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                Discussions on the synthesis of LSD
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   Kaff         posted 05-16-98 07:36 PM CT (US)
                ----------------------------------------------------------
                It just occurred to me that noone ever mentions acid. I
                have Fester's book Practical LSD Manufacture but that's
                about as practical as buying a wheat farm just to make
                acid. Yeah right Hawaiin Baby woodrose seeds and morning
                glory seeds have some lysergic acid, but why aren't there
                any new methods?

   drone 342    posted 05-16-98 07:50 PM CT (US)
                ----------------------------------------------------------
                I agree, Fester's LSD book was a major disappointment --
                yet one more reason to loath the guy. There is an
                advancement, one which Fester didn't include, which is
                the use of POCl3 as a dehydrating reagent in the
                condensation of lysergic acid with diethylamine. Check
                out Rhodium's page, as well as hyperreal for more info on
                this new developement.

                The wierdest part about it is that it was developed by
                our friends over at the Edgewood Arsenal in Maryland
                during the mid-seventies -- the good people who lead the
                world in cutting-edge chemical warfare technology and
                supply the intelligence community with all the wierd shit
                they use. These are the same folks who stockpiled QNB in
                multi-kilo quantities right into the eighties, as well as
                the freaky things they don't tell anyone about. Some day,
                I want a tour of that place.

                Anyways, the important thing to keep in mind, which
                really shows yet again how much Fester talks out of his
                ass, is that all the seeds, fungi, and other biomass is
                NOT the way to allocate your lysergic compounds for this
                reaction. Anybody who makes it on a big scale is using
                most liekely ergot alkaloids from a commercial source --
                foreign pharmacy companies, etc. Its not that hard to get
                your hands on an ounce or two of ergotamine or ergonovine
                if you put your noggin to it. Hell, even bromocryptine
                will work (remove the bromine by maing the grignard out
                of it, then hydrolyzing it. As long as its done gently,
                no funky additions, olgermizations or whatever, will
                happen.)

                I've been waiting for someone to bring this subject up.
                Ask and you shall recieve.

                -drone #342

   KrZ          posted 05-17-98 03:28 AM CT (US)
                ----------------------------------------------------------
                Whats wrong with Hawaiin Baby Woodrose? When your making
                something where 1 dose=50 micrograms a pound of HWBR goes
                a long ways... Does fester talk about culturing as a
                source in an incubator?

   Fan of       posted 05-17-98 03:24 PM CT (US)
   Shulgin
                ----------------------------------------------------------
                IMHO culturing the ergot fungus in the best method by far
                for producing LSD. Even someone with absolutely no
                knowledge of microbiology can culture ergot. And as to
                obtaining the fungus, it can be found in most large
                fields of rye. This is no joke, wait just until harvest
                time and go out and have a look for the 'heads'. The
                beauty of growing the Claviceps is that you can keep it
                alive for ever if you are careful, and thus have an
                almost never ending supply of raw material.

                It is worth noting, that this is the method that most
                illegal acid labs operate (look up operation Julie in the
                UK!). Even producing acid on a small scale requires you
                to prepare shit loads of the precursors, because even
                working under red light at low temperatures and low
                humidity does not have that great an effect on keeping
                yields high (a 20% yield in LSD manufacture is considered
                a great success). Remember LSD is inherantly unstable!

                Anyway - LSD synthesis, Claviceps cultivation etc are one
                of the most talked about drug manufacturing methods on
                the net. Have a good long search around!

                Peace, Love and empathy

                Fan of Shulgin

   drone 342    posted 05-17-98 11:15 PM CT (US)
                ----------------------------------------------------------
                I'm telling you guys, mushroom cultivation IS NOT where
                its at! As far as I can tell, this is not as common of a
                procedure as people believe. Why? Ever look at the amount
                of solvents entailed in extracting the stuff? This is a
                way too involved process that uses far too many
                resources. MAYBE there's some lab that does this, but
                it's just not practical. Besides, this bioproduction
                entails the chemist mastering a whole bunch more skills
                than the tricky ones already required.

                I stand by my procedure as THE ONE TRUE WAY(tm), or at
                least the best of the one true ways. Think about it:
                Bromocryptine into bromolysergic acid. Bromolysergic acid
                into bromolysergic acid diethylamide. Bromolsyergic acid
                diethylamide into its respective grignard reagent.
                Grignard reagent decomposition into LSD. Add a dash of
                tartaric acid, and chromatograph it. All pretty simple
                procedures -- relatively speaking.

                Bromocryptine is easy to get in reasonable quantities.
                Other ergot alkaloids are also available, and would alow
                the chemist to skip a debromination step or two as well.

                While some believe that LSD is only worthwhile on a
                mega-huge scale of ounces at a time, I contend that using
                the sources I suggest, that a gram-size batch would still
                be a very attractive endevor.

                HBWR seeds might be a decent way to go, I agree, but I
                prefer pill extracting any day. Considering also the
                price and notriousness of this as a source, other sources
                should be investigated more thotoughly. How much does a
                kilo of seeds go for nowadays?

                Still, here's another source. Grain companies have a lot
                of fancy-shmancy equiptment I've been told, soley to
                remove claviceps from our food supply. This means that
                every harvest season, your local grain elevator has got
                pounds of ergot-ladden grain that they normally throw
                away. This I heard from a friend of mine who worked in a
                grain elevator -- lost contact with him since my chemical
                skills were upgraded. This is worth some investigating.

                Anyways, I agree that far too little research is being
                done into these matters, and I'd like to see more
                discussion of the chemistry of Hoffmann's baby. The
                chemistry IS above kitchen production conditions, but not
                out of reach for the semi-elite of The Hive's Chemical
                Guard. By eliminating the riduculous, over-complicated
                bullshit procedures out there, and replacing them with
                simpler, more practical means, the small circle of people
                willing-and-able to perform this most sacred of chemistry
                is widended considerably.

                May The Force be with you all,

                -drone #342

   KrZ          posted 05-18-98 12:40 AM CT (US)
                ----------------------------------------------------------
                Drone, c'mon, we are not talking about mushrooms here,
                wake up son... Mushrooms growing right on top of rye
                plants, that would look prety silly.. All you need is a
                sample, some .2% agar plates and some sterile technique,
                not exactly skill-requiring stuff..

                (don't mind the teasing D ;-)

   drone 342    posted 05-18-98 09:22 AM CT (US)
                ----------------------------------------------------------
                KrZ said:

                Drone, c'mon, we are not talking about mushrooms here,
                wake up son... Mushrooms growing right on top of rye
                plants, that would look prety silly.. All you need is a
                sample, some .2% agar plates and some sterile technique,
                not exactly skill-requiring stuff..

                KrZ:

                Sorry, I suffer from a mild case of irony deficiency, and
                so its hard for me to tell when folks are pulling my leg.
                I wholeheartedly aprove of and endorse mushroom
                cultivation -- provided it is of my favorite
                basidiomycetes genus that starts with the letter "p".

                However, I think you'll discover claviceps is harder than
                you think. Ever try to get a pure culture of that stuff?
                If you go through any of the research collections or
                biotech companies, you're going to have to fill out more
                paperwork than you'd believe -- not because its laden
                with ergot goodness, but because its considered a
                agriculturally harmful organism. It's about as involved
                as filling out forms for the purchasing of an
                encapsulating machine. If you choose to isolate your own
                strain frm the field, good luck. You got a 2-month or so
                window of time to collect it, and then comes the
                isolation process. Then once you have pure claviceps,
                you're going to have to isolate a decent-producing
                heterokaryote from your collection, which you may or may
                not have. Once you manage THAT, then comes the perti dish
                phase, followed by the initial submerged culture for
                producing seed stock, then finally the large-scale
                submerged culture to yield a a sludge of filaments you
                gotta strain out, dry, then extract.

                Yuck. There are a lot of professional folks out there
                who's entire days, nay, entire *careers* relovle around
                ergot production. I rather rely on the fruits of their
                labor and save all the schmassle that this project would
                otherwise entail.

                Think about it. I honestly feel the main detractor from
                more people producing LSD is this ergot culturing myth.
                Yeah, everyone says "Boy, I sure wish I could make some
                good acid. All I gotta do is get a chemistry degree under
                my belt, get a good lab space, and on top of that, raise
                a culture of some fucked-up saprophytic fungus that'll
                give me gangreen in the process." This is obviously
                daunting. If you disagree and say its not too much of a
                bother, then why aren't more people kicking out kilos of
                "L"? What I'm proposing is that this fungus cultivation
                idea is more of a detriment to acid production than an
                advantage. Just extract the shit from pills, or go to the
                third world where the stuff is cheap, and you can buy it
                in its straight uncut powder form for pharmaceutical
                outlets (there are several countries where you can do
                this when you know a good pharmacist and have the cake to
                do some bribing; believe me, I've looked.)

                As simple as ergot cultivation sounds, there's plenty of
                reasons its not done commonly.

                -drone #342

   drone 342    posted 05-18-98 09:25 AM CT (US)
                ----------------------------------------------------------
                Oh yeah, and I almost forgot. With bromocriptine, you can
                do that grignard degredation process as your first couple
                steps; this wil cut down on the amounts of POCl3 and Et2N
                required in the amidation and save you precious
                resources. Grignards don't readily add to amides, so you
                can take advantage of that.

                -drone #342

   drone 342    posted 05-20-98 09:24 AM CT (US)
                ----------------------------------------------------------
                Okay, so of available precursors for acid, we got:

                *HBWR
                *Ipomoea sp.
                *Claviceps sp.
                *Ergot alkaloid pills (ergotamine, ergonovine, etc.)
                *bromocriptine
                *a few other misc. plants

                Seems to me the chemistry and methodology is pretty
                cut-and-dry -- the main problem is precursor aquisition.
                So what other exciting sources might be out there for the
                ergoloid ring?

                -drone #342

   Commodium    posted 05-20-98 11:56 AM CT (US)
                ----------------------------------------------------------
                For what it's worth, cheapest I've seen for HBWR on the
                'Net is this place . . .

                Blue Ridge Garden
                P.O. Box 52
                Mint Spring, VA 24463
                no catalogue, free shipping

                $180/lb. ($396/key)

   drone 342    posted 05-20-98 12:25 PM CT (US)
                ----------------------------------------------------------
                Y'know, it's been years since I looked at HBWR seeds, and
                I can't remember for the life of me a good reference
                source describing the alkaloid concentraion in these
                buggers. Yes, there are FAQ's, but what I want is a good,
                academic journal article listing the juicy details.

                There's a good list at paranoia describing a number of
                sources for these seeds -- there's a Hawaiian place
                selling them for $80/8 oz.

                So, considering the nightmarish pile of ref's I've listed
                lately for the Hive, I'm gonna let someone else this time
                get the goods. I just KNOW someone out there has a ref
                like the one I'm looking for hanging on their
                refridgerator door.

                -drone #342

   drone 342    posted 05-20-98 01:30 PM CT (US)
                ----------------------------------------------------------
                Actually, I just stumbled across the articles I was
                looking for:

                J of the AOAC vol 53:1 123-127 (1970)
                J. Pharm. Sci. 62:4 588-591 (1973)

                -drone #342

   Commodium    posted 05-20-98 02:17 PM CT (US)
                ----------------------------------------------------------
                Yeah, looks like (according to that Journal of the AOAC
                article) Hawaiian Baby Wood Rose is 0.04 to 0.30 % LSA,
                by weight.

   drone 342    posted 05-20-98 06:56 PM CT (US)
                ----------------------------------------------------------
                Incidentally, I looked into the possible utilization of
                sleepy grass, butit looked like it was full of all sorts
                of other alkaloid garbage aside from lisergic acid and
                its amides. Chanoclavines, Pyridines, etc. This might be
                a good source if anybody knows a good way of separating
                the wheat from the chaff in this case. What else besides
                HPLC will do the trick? (I have an HPLC machine for my
                amusement, but I can only do tiny volumes; besides, half
                the point of this research is figuring out ways of doing
                this kind of stuff successfully garage-style rather than
                just in the lab.)

                Also, does anybody else harbor the same loathing for
                Fester and his piece-o-shit-excuse-for-an-acid-book as I
                do? I mean, he completely missed the POCl3 method, and
                left "method X" a mystery (even though its probobly just
                as full of shit as the rest of the book.) In addition, he
                mistakenly thought propionic anhydride had something to
                do with acid chemistry, and then didn't even give a
                particularily meaningful synthesis for it. All his
                methods looked like rehashes of patents from the earlier
                part of this century (available in half a dozen other
                publications already,) and the only lysergic acid source
                he offers is buying a goddam wheat farm and raising a
                crop of moldy rye grain! Even his claviceps raising would
                take over a year to accomplish!

                So, his book only would be practical for a farmer with a
                couple years on his hands, a few 55-gallon barrels of
                tech-grade solvents, a lab full of large-scale equiptment
                for advanced organic chemical procedures, and some rather
                extensive training in organic chemistry. If a person had
                all those resources available to them at the same time,
                they'd be an idiot if they couldn't find a better way of
                going about things than that.

                -drone #342

   buzzz        posted 05-20-98 07:56 PM CT (US)
                ----------------------------------------------------------
                i have'nt looked over it a great deal but, the book
                PSYCHEDELIC CHEMISTRY by michael valentine smith gives
                detailed info on lysergic acid and extractions for ergot
                extraction from HBWS and states that the seeds yield 7mg
                alkaloids/100 g of seeds and that thru the usual steps to
                reach the end point of lsd that you get roughly 1g LSD /
                kg of seed .the book can be ordered from loompanics

   drone 342    posted 05-20-98 08:41 PM CT (US)
                ----------------------------------------------------------
                Got a copy of that one already; what library would be
                complete without MVS's book? Nothing too
                earth-shattering, but still I like it; there's an aura of
                honesty to it that you don't see in many other
                underground drug books. MVS is sure no formally-trained
                chemist, but at least he knew how to operate a copying
                machine and give credit where it was due.

                Your numbers don't add up.
                (7mgergot/100gHBWR)X(1000g/1kg) does not equal even 1g of
                ergot, but I get the general gist of it. I'll give it a
                look-see. Thanks for the tip. Considering that a kilo can
                be boughten for around $300-$400 dollars, it looks like
                it would almost be a good investment (I prefer the
                chemistry of drugs where the profit margin is closer to
                95-99% rather a mere 75-80%, but hey, its acid.)

                -drone #342

   KrZ          posted 05-21-98 02:26 AM CT (US)
                ----------------------------------------------------------
                LSD Manufacture

                Illegal LSD Production

                LSD has been manufactured illegally since the 1960?s. A
                limited number of chemists, probably less than a dozen,
                are believed to be manufacturing nearly all of the LSD
                available in the United States. Some of these manufacturers
                probably have been operating since the 1960's.

                LSD manufacturers and traffickers can be separated into
                two groups. The first, located in northern California, is
                composed of chemists (commonly referred to as 'cooks') and
                traffickers who work together in close association; typically,
                they are major producers capable of distributing LSD
                nationwide. The second group is made up of independent
                producers who, operating on a comparatively limited scale,
                can be found throughout the country. As a group, independent
                producers pose much less of a threat than the northern
                California group inasmuch as their production is intended
                for local consumption only.

                Drug law enforcement officials have surmised that LSD
                chemists and top echelon traffickers form an insider's
                fraternity of sorts. They successfully have remained at
                large because there are so few of them. Their exclusivity
                is not surprising given that LSD synthesis is a difficult
                process to master. Although cooks need not be formally
                trained chemists, they must adhere to precise and complex
                production procedures. In instances where the cook is not
                a chemist, the production recipe most likely was passed on
                by personal instruction from a formally trained chemist.  
                Further supporting the premise that most LSD manufacture is 
                the work of a small fraternity of chemists, virtually all
                the LSD seized during the 1980's was of consistently high
                purity and sold in relatively uniform dosages of 20 to 80
                micrograms.

                LSD commonly is produced from lysergic acid, which is
                made from ergotamine tartrate, a substance derived from
                an ergot fungus on rye, or from lysergic acid amide, a
                chemical found in morning glory seeds. Although
                theoretically possible, manufacture of LSD from morning glory
                seeds is not economically feasible and these seeds never
                have been found to be a successful starting material for
                LSD production. Lysergic acid and lysergic acid amide are
                both classified in Schedule III of the Controlled Substances
                Act. Ergotamine tartrate is regulated under the Chemical
                Diversion and Trafficking Act.

                Ergotamine tartrate is not readily available in the
                United States, and its purchase by other than established
                pharmaceutical firms is suspect.  Therefore, ergotamine
                tartrate used in clandestine LSD laboratories is believed
                to be acquired from sources located abroad, most likely
                Europe, Mexico, Costa Rica, and Africa.11 The difficulty
                in acquiring ergotamine tartrate may limit the number of
                independent LSD manufacturers. By contrast, illicit
                manufacture of methamphetamine and phencyclidine is
                comparatively more prevelant in the United States because,
                in part, precursor chemicals can be procured easily.

                Only a small amount of ergotamine tartrate is required to
                produce LSD in large batches. For example, 25 kilograms
                of ergotamine tartrate can produce 5 or 6 kilograms of pure
                LSD crystal that, under ideal circumstances, could be
                processed into 100 million dosage units, more than enough to
                meet what is believed to be the entire annual U.S. demand
                for the hallucinogen. LSD manufacturers need only import a
                small quantity of the substance and, thus, enjoy the advantages
                of ease of concealment and transport not available to
                traffickers of other illegal drugs, primarily marijuana
                and cocaine.

                Cooking LSD is time consuming; it takes from 2 to 3 days
                to produce 1 to 4 ounces of crystal. Consequently, it is
                believed that LSD usually is not produced in large
                quantities, but rather in a series of small batches.
                Production of LSD in small batches also minimizes the loss of
                precursor chemicals should they become contaminated during
                the synthesis process.

                LSD crystal produced clandestinely can be as much as 95-
                to 100-percent pure. At this purity-and assuming optimum
                conditions during dilution and application to paper-1 gram
                of crystal could produce 20,000 dosage units of LSD.
                However, analysis of LSD crystal seized in California over
                the past 3 years revealed an average purity of only 62
                percent. Moreover, LSD degrades quickly when exposed to
                heat, light, and air and is most susceptible to degradation
                during the application process and once it is in paper form.
                As a result, under less than optimal, real-life conditions,
                actual yields are significantly below the theoretically
                possible yield: 1 gram of LSD crystal genarally yields
                10,000 dosage units of LSD, or approximately 10 million
                dosage units per kilogram.

                Over the past 30 years, the traditional dilution factor
                for manufacturing LSD has been 10,000 doses per 1 gram of
                crystal. Therefore, dosage units yielded from high-purity
                (95- to 100-percent pure) LSD crystal would contain 100
                micrograms. However, dosages currently seen contain closer
                to 50 micrograms. This discrepancy stems in part from
                production impurities: during the sythesis process,
                manufacturers generally fail to perform a final 'clean-up'
                step to remove by-products, thereby lowering the crystal's
                purity. Further, though average purity of tested LSD crystal
                samples is, as noted, 62 percent, the average potency of
                doses analyzed is approximately 50 micrograms rather than 62
                micrograms, as would be expected. The diminished potency
                can be attributed to distributors who, when applying the
                crystal to paper, often 'cheat' by diluting 1 gram of
                crystal to produce up to 15,000 or more dosage units.

                Pure, high-potency LSD is a clear or white, odorless
                crystalline material that is soluble in water. It is
                mixed with binding agents, such as spray-dried skim milk,
                for producing tablets or is dissolved and diluted in a
                solvent for application onto paper or other materials.
                Variations in the manufacturing process or the presence of
                precursors or by-products can cause LSD to range in color
                from clear or white, in its purest form, to tan or even
                black, indicating poor quality or degradation. To mask
                product difficiencies, distributors often apply LSD to
                off-white, tan, or yellow paper to disguise discoloration.

                At the highest levels of the traffic, where LSD crystal
                is purchased in gram or multigram quantities from wholesale
                sources of supply, it rarely is diluted with adulterants, a
                common practice with cocaine, heroin, and other illicit
                drugs. However, to prepare the crystal for production in
                retail dosage units, it must be diluted with binding agents
                or dissolved and diluted in liquids. The dilution of LSD
                crystal typically follows a standard, predetermined recipe
                to ensure uniformity of the final product. Excessive dilution
                yields less potent dosage units that soon become unmarketable.

                LSD crystal usually is converted into tablet form ('microdots'
                that are 3/32 inch or smaller in diameter), thin squares of
                gelatin ('window panes'), or applied to sheets of prepared
                paper (blotter paper-initially used as a medium-has been
                replaced by a variety of paper types).  LSD most frequently 
                is encountered in paper form, still commonly referred to as
                blotter paper or blotter acid. It consists of sheets of paper
                soaked in or otherwise impregnated with LSD. Often these
                sheets are covered with colorful designs or artwork and
                are usually perforated into one-quarter inch square,
                individual dosage units.

   KrZ          posted 05-21-98 02:48 AM CT (US)
                ----------------------------------------------------------
                Michael Valentine Smith: Psychedelic Chemistry

                From pages 105-107:

                The Culture and Extraction of Ergot Alkaloids

                Make up a culture medium by combining the following
                ingredients in about 500 milliliters of distilled water
                in a 2 liter, small-neck flask:

                Sucrose .................................... 100 grams
                Chick pea meal .............................. 50 grams
                Calcium nitrate .............................. 1 gram
                Monopotassium phosphate ...................... 0.25 grams
                Magnesium sulphate ........................... 0.25 grams
                Potassium chloride ........................... 0.125 grams
                Ferrous sulphate heptahydrate ................ 8.34 milligrams
                Zinc sulphate heptahydrate ................... 3.44 milligrams

                Add water to make up one liter, adjust pH 4 with ammonia
                solution and citric acid. Sterile by autoclaving.

                Inoculate the sterilized medium with Claviceps purpurea
                under sterile conditions, stopper with sterilized cotton
                and incubate for two weeks periodically testing and
                maintaining pH 4. After two weeks a surface culture will
                be seen on the medium. Large-scale production of the fungus
                can now begin.

                Obtain several ordinary 1 gallon jugs. Place a two-hole
                stopper in the necks of the jugs. Fit a short (6 inch)
                glass tube in one hole, leaving 2 inches above the stopper.
                Fit a short rubber tube to this.  Fill a small (500
                milliliter) Erlenmeyer flask with a dilute solution of
                sodium hypochlorite, and extend a glass tube from the rubber
                tube so the end is immersed in the hypochlorite. Fit a long,
                glass tube in the other stopper hole. It must reach near
                the bottom of the jug and have about two inches showing
                above the stopper. Attach a rubber tube to the glass tube as
                short or as long as desired, and fit a short glass tube to 
                the end of the rubber tube. Fill a large, glass tube (1 inch
                x 6 inches) with sterile cotton and fit 1-hole stoppers in
                the ends.  Fit the small, glass tube in end of the rubber
                tube into 1 stopper of the large tube. Fit another small
                glass tube in the other stopper.  A rubber tube is connected
                to this and attached to a small air pump obtained from a
                tropical fish supply store. You now have a set-up for pumping
                air from the pump, through the cotton filter, down the long
                glass tube in the jug, through the solution to the air
                space in the top of the jug, through the short glass tube,
                down to the bottom of the Erlenmeyer flask and up through
                the sodium hypochlorite solution into the atmosphere. With
                this aeration equipment you can assure a supply of clean air
                to the Claviceps purpurea fungus while maintaining a sterile
                atmosphere inside the solution.

                Dismantle the aerators. Place all the glass tubes, rubber
                tubes, stoppers and cotton in a paper bag, seal tight with
                wire staples and sterilize in an autoclave.

                Fill the 1-gallon jugs 2/3 to 3/4 full with the culture
                medium and autoclave.

                While these things are being sterilized, homogenize in a
                blender the culture already obtained and use it to inoculate
                the media in the gallon jugs. The blender must be sterile.
                Everything must be sterile.

                Assemble the aerators. Start the pumps. A slow bubbling
                in each jug will provide enough oxygen to the cultures. A
                single pump can, of course, be connected to several filters.

                Let everything sit a room temperature (25 C) in a fairly
                dark place (never expose ergot alkaloids to bright light -
                they decompose) for a period of ten days.

                After ten days adjust the culture to 1% ethanol using 95%
                ethanol under sterile conditions. Maintain growth for another
                two weeks.

                After total of 24 days growth period the culture should
                be considered mature. Make the culture acidic with tartaric
                acid and homogenize in a blender for one hour.

                Adjust to pH 9 with ammonium hydroxide and extract with
                benzene or chloroform/iso-butanol mixture.

                Extract again with alcoholic tartaric acid and evaporate
                in a vacuum to dryness. The dry material in the salt (i.e.,
                the tartaric acid salt, the tartrate) of the ergot alkaloids,
                and is stored in this form because the free basic material is
                too unstable and decomposes readily in the presence of light,
                heat, moisture and air.

                To recover the free base for extraction of the amide of
                synthesis to LSD, make the tartrate basic with ammonia to pH
                9, extract with chloroform and evaporate in vacuo.

                If no source of pure Claviceps purpurea fungus can be
                found, it may be necessary to make a field trip to obtain
                the ergot growths from rye or other cereal grasses. Rye
                grass is by far the best choice. The ergot will appear as a
                blackish growth on the tops of the rye where the seeds are
                and are referred to as "heads of ergot." From these heads
                of ergot sprout the Claviceps purpurea fungi. They have
                long steams with bulbous heads when seen under a strong
                glass or microscope. It is these that must be removed
                from the ergot, free from contamination, and used to
                inoculate the culture media. The need for absolute sterility
                cannot be overstressed. Consult any elementary text on
                bacteriology for the correct equipment and procedures.
                Avoid prolonged contact with ergot compounds, as they are
                poisonous and can be fatal.

                ----------------
                The whole part with the pump is unecessary, you can get
                micropore 1-gallon jugs from www.fungi.com, and alot of
                the gear you would need, obtaining a pure strain sounds
                like the tricky part, culturing and selection of
                pure-looking samples a couple times should do it.. LSD
                must be synthesized, it's such a beautiful molecule...

   Piglet       posted 05-21-98 12:30 PM CT (US)
                ----------------------------------------------------------
                Fan of Shulgin: I checked out the 'Operation Julie' book
                and it says that the Ergot compounds were ALL bought.
                Initially by simply driving to Switzerland and paying
                cash (those were the days!) and later using fake
                companies and from underground sources (Brotherhood of
                Eternal Love with Leary et all).
                I have never read of any large LSD manufacturers making
                there own. It is quite a skill & is quite dangerous
                (ergot IS classed as a poison, do you like your
                extremeties? Do you want them to go black and drop off?
                Don't try growing ergot without knowing the safety rules)

                Someone I know was in prison with Kemp (the Julie
                main-man) and Kemp is a 1 in a million brainiac.

                Ergot compounds appear in certain prescription migraine
                medications (all made by Sandoz, fancy that!)

                The book 'Operation Julie' has a few pictures of the
                chemistry setup. It was pretty involved stuff. One small
                hilight was a brown bottle featured slap-bang in the
                middle of one picture. It said 'NaNO2'. Fester says that
                this 'might' be a replacement for acetyl-acetone. It is.
                THAT was the Method-X bit. It's not even a secret.

   drone 342    posted 05-21-98 04:54 PM CT (US)
                ----------------------------------------------------------
                Here's a thought:

                What about using DCC as your dehydrating reagent for
                forming an amide bond? High yields and low temps means
                better product in larger quantities. Ref

                Encyclopedia for Organic Synthesis, Paquett,L.A., Ed;
                Wiley, 1995; vol. 3, p. 1731

                also check your Merck (of course)

                Much of the fancy-schmancy technology devoted to peptide
                synthesis is equally applicable in this situation as
                well. There's a ton of ways to go from an acid to an
                amide, and its good to have as many as possible in one's
                repetoire.

                in a synthetic mood,

                -drone #342

   drone 342    posted 05-21-98 05:31 PM CT (US)
                ----------------------------------------------------------
                oh yeah, DCC is "DiCyclohexylCarbodiimide".

                Structure:

                (C6H12)-N=C=N-(C6H12)

                Th reaction converts this to dicyclohexylurea.

                -drone #342

   KrZ             posted 05-22-98 12:47 AM CT (US)
                ----------------------------------------------------------
                JLF sells pure claviceps purpea 1 gm for 10.00.

   drone 342    posted 05-22-98 09:50 AM CT (US)
                ----------------------------------------------------------
                Re: Claviceps. That doesn't sound like too good of a
                deal. Do they have better prices when you buy in bulk?
                Even at half the price, that really isn't too good a
                deal. Considering the tiny percentage of ergot alkaloids
                in a gram, then considering how much less you have after
                hydrolyzing off those useless peptides, and how much less
                you have still after the dehydration of the acid with
                ethylamine, ten dollars is way more than street prices.
                This isn't even counting in labor as a cost (most
                chemists I know like to get paid.)

                -drone #342

   josh         posted 05-22-98 02:07 PM CT (US)
                ----------------------------------------------------------
                Hey drone,would you post a synth. for lsd using
                bromocryptine.This synthesis that you have briefly
                described is very interesting.This bee would greatly
                appreciate it.

   Ritter       posted 05-22-98 08:40 PM CT (US)
                ----------------------------------------------------------
                Drone,

                I'm no expert on Grignards, however do you really feel
                you could get the -Br to react w/ Mg to make the
                Grignard? My experience has been that its pretty freakin'
                difficult to make tender complicated multi-cyclic
                molecules such as bromocryptine undergo Grignard
                formation. I only skimmed your comments above and may be
                reiterating what you stated but I think the best way to
                go about this would be to hydrolyze off the peptide
                garbage leaving bromo lysergic acid and then subject this
                to Grignard's reaction. I think the appropriate time to
                form the amide is after the Grignard because a carboxyl
                group will probably be less reactive than an amide group
                towards the Grignard.

   Fan of          posted 05-23-98 06:14 AM CT (US)
   Shulgin
                ----------------------------------------------------------
                Sure, you may only get a small amount for $10 - but it is
                a living organism, and it reproduces quickly! Just drop
                some onto an agar plate, come back the next day and see
                what I mean!

                You only need a small amount to get started, the amount
                you finally grow is limited only by the space you can set
                aside for the cultures to grow!

   quirks       posted 05-23-98 08:29 AM CT (US)
                ----------------------------------------------------------
                fyi - your local country vet will have a couple of boxes
                of egrotvine (or whatever it is that's used for
                birthing), amounting to a couple of grams.

   KrZ             posted 05-24-98 01:36 AM CT (US)
                ----------------------------------------------------------
                Like F.O.S. said it comes as a living sample on a dish,
                then you could use that procedure for culturing...

   drone 342       posted 05-24-98 01:06 PM CT (US)
                ----------------------------------------------------------
                Ritter,

                Yes, Grignard will work wonders in this case, and no, it
                actually is easy to get it to do it. All that multicyclic
                studd simply doesn't appeal to the grignard substituent
                -- its looking for an electron-deficient site labile and
                with nowhere to run to. Amides are surpisingly sturdy to
                these condsitions, and will not readily react at all. As
                far as I see it, that would really be the only concern
                (regarding the carbonyls found therin.)The reason for
                this is that the nitrogen is electron donating, whereas
                in any other carbonyl, it doesn't have this luxury, and
                will react readliy with a Grignard. Conditions are a
                snap, just a nice dry ether soultion or Benzene solution
                (with light being thoroughly eliminatined from the
                envronment around the flask) of the free base of your
                ergot caompound in question will do. If you're still
                worried about that reaction affecting the peptide, just
                save it for the last step -- make bromo-LSD, then do it.
                I guaruntee that the amide will be safe.

                Quirks,

                Thank you. This is the useful type of information we need
                buckets of if we want to end the war on drugs (my
                strategy: an all-out assault; a psychedelic blitzkrieg.
                Hey, now that's a catchy phrase!)

                -drone #342

   drone 342       posted 05-24-98 02:55 PM CT (US)
                ----------------------------------------------------------
                Fan of Shulgin,

                Where can you get a living 1-gram clean specimen of
                claviceps purpurea? Are you sure its alive? How do you
                know this works, or is this strictly speculation?

                Josh,

                Tell you what; I'll give the ref's, and anybody with the
                resources to actually perform this should also have
                plenty of access to the library. Actually, all you need
                is a copy of a decent lab manual describing the synthesis
                of grignard reagents, and follow the general guidelines
                for producing a Grignard intermediate. Then, add water.
                You now have ergocriptine. Hydrolyze it and condense with
                diethylamine according to the proceedures listed in
                TiHKAL.

                Alternatively, one could use DCC. From the Encyclopedia
                of Reagents for Organic Synthesis:

                Typically, DCC (1.1 equiv) is added to a concentrated
                solution (0.1-1.0M) of the carboxylic acid (1.0 equiv),
                amine (1.0 equiv), and catalyst (when used) in methylene
                chloride or acetonitrile at 0 deg C. The hydrated DCC
                adduct, dicyclohexylurea (DCU), quickly precipitates and
                the reaction is generally complete within 1 h at rt..."

                Downsides: THF and DMF screw things up by slowing things
                down and ecouraging the production of side-products, as
                well as racemizing the carboxylic acid. The other
                downside is in some solvents, a trace of DCU can disolve
                in with your product, requiring purification (nothing
                flash chromatography wouldn't take care of quite easily,
                which you have to do anyways if you want to be a good
                person.)

                further refs:

                JACS 1955, 77, 1067
                Chem & Ind (London) 1955, 1087
                Badanszky, M. Peptide Chemistry: A Practical Textbook;
                Springer: NY, 1988
                JOC 1971, 36,1909

                -drone #342

   Piglet       posted 05-26-98 09:59 AM CT (US)
                ----------------------------------------------------------
                Fan Of Shulgin: When I typed about the dangers of ergot,
                I meant to to guy producing it. The actual amount of
                ergot needed to produce 'St. Antonys Fire' immediately
                seem quite low. It was estimated from the last outbreaks
                (after WW2 when people were starving and would eat
                ANYTHING including infested rye) that about 30mg causes
                SEVERE reactions. I know you would never ingest such
                amounts of ANY substence in a lab, but growing your own
                ergot is not a lab technique. I did check out that old
                chestnut about growing in culture. Most of the
                researchers had little success. I think it CAN be
                produced in culture, but only by someone who REALLY knows
                there stuff. Sandoz grow rye to this day!

   drone 342    posted 06-10-98 09:29 PM CT (US)
                ----------------------------------------------------------
                Piglet, where did you get this information about Sandoz?
                As far as I know, Claviceps is one of those organisms
                that researchers have spent a lot of time, money, and
                energy in getting it to grow in submerged culture on a
                large scale -- and have come up with a successful means
                of doing so. I've heard some similar things in
                publications from times past, but I suspect that in
                modern industry, the transition has been made.

                -drone #342

   Cherrie      posted 06-11-98 06:32 PM CT (US)
   Baby
                ----------------------------------------------------------
                "Where can you get a living 1-gram clean specimen of
                claviceps purpurea?"

                During late summer have a look at the Rye grass in the
                local park. You'll notice a purple-brown "ear" growing on
                the rye seeds - this stuff is Claviceps purpurea. It
                grows in my back garden. If you have some experience with
                shrooms this is easy to grow. The big catch is that
                nearly all the LSA producing ergot has been from
                particular strains which you'll have to get from a lab
                that stocks pure cultures. I don't think wild ergot would
                work when making LSA's. I've been told that you can grow
                the ergot (easily) but it won't make LSA unless it's the
                right strain!

                Are there any biochemists out there who know the answer
                to this one way or another?

   Commodium    posted 06-11-98 07:17 PM CT (US)
                ----------------------------------------------------------
                Update...an even cheaper place for HBWR (LSA) is:

                Herben Shaman (via Lycaeum)
                4 oz $42
                8 oz $75
                1 lb $135
                1 kg $225



--------------------------------------------------------------------------------
Forest Gump (Dec. 24, 1997 at 19:15) - Hive

The book that you refer to "Practical LSD Manufacture" by Uncle Fester, now in 
its 2nd Ed. isn't completely about LSD, although from the title one could get 
that impression. The first edition contianed 115 pages, of which only about 70 
pages actually had anything to do with LSD synthesis, the rest mostly about 
Fester's pet project: TMA-2 synthesis. The second edition contains 142 pages, 
almost all the extra pages going to his pet project -- which now consumes about 
halve the book -- while the LSD portion remains virtually unchanged (all the 
errors and mistakes of the first edition were remarkably well preserved into 
the second). A naive person could be forgiven for mistakenly thinking the book 
of being just a vehicle for his pet project -- but of course we know better.

Before I list just some of those errors let me preface it with this: it is 
obvious that not only does Fester not have any practical experience with 
Lysergic chemistry, but that he is also confused by it.

1.) Isomer Confusion. In chapter 4 Fester makes repeated mistakes as to 
chirality. On page 24, in reference to the anhydrous hydrazine degradation 
method, he tells us that this procedure produces very little iso- compound, 
when in fact it produces predominately iso- material. On page 25 he informs 
us of the importance of maintaining anhydrous conditions to avoid getting 
racemic product -- on further reading it is obvious that by "racemic" he 
means iso/normal mixtures, as nowhere is there to be found any reference 
to the l (levo) compound.

The older hydrazine hydrate method produced a 1/1 mixture of d and l compounds; 
the l compounds are inactive and represent a total loss, as there is no 
convenient method to convert them into the desired d compound. The anhydrous 
hydrazine method is a newer improvement upon this which avoids the l compound, 
but it still gives about 2/3 of the iso- compound which is also inactive; 2/3 
inactive product sounds real bad, but it's not nearly as bad as the older 
method because the iso- compound is easily isomerized into the active compound 
in about 2/3 yield. When Hofmann refers to this new method as not producing any 
"racemic" material what he means is that it doesn't produce any of the useless 
l compound, not that it doesn't produce iso- compound.

Also, the amidation procedure he gives in the same chapter produces some iso- 
compound, although nowhere does he mention that. Indeed, from reading the 
purifacation procedure, he seems to think that this amidation method also 
preserves chirality.

2.) Continuum Error. The first paragraph on page 27 (i.e., "Both of these 
choices are really very poor, ...") picks up from nowhere, and we're left to 
wonder what he's refering to. Chalk this one upto bad proofreading (this is 
Loompanics we're talking about after all).

3.) Outdated Methods. The four amidation methods in the book have long since 
been superseded by the phosphorus oxychloride in chloroform method, which is 
not in the book.

4.) Method X. In the book a big deal is made about his erroneous discovery of 
a "superior" LSD method which he calls "method x". I'll spare you all the 
convoluted details and inane logic of how he came about this "discovery" except 
for this one statement of his: "Note that propionic anhydride is a listed 
chemical under the Chemical Diversion Act, with a reporting threshold of 1 gram. 
There is only one substance in the field of clandestine drug manufacture where 
1 gram is a significant amount -- LSD"

I'm sure not a few DEA chemists must have laughed there ass off after having 
read that. Propionic anhydride is used to make fentanyl and its analogues. 
Some fentanyl analogues are 10 times more potent than LSD!!!!

And that is just some of the errors contained within that book. And with that 
I'll leave you, hopefully a little bit more knowlegable. 

-- Forest Gump

--------------------------------------------------------------------------------

Thanks for the info.

FX (Dec. 25, 1997 at 09:51):

Hey, thanks a lot. You seem to know quite a bit about LSD chemistry. I'm sure 
that Fester's book has some errors, but I am not aware of any other book in 
existence on practical LSD manufacture. Are you? It is amazing how few people 
know anything about LSD synth, apparently it is the hardest recreational drug 
to manufacture of them all, much much harder than ectacy or meth. Why is this? 
How should someone go about learning about LSD manufacture assuming that they 
don't have PhDs in chemistry? According to DEA, almost all of the LSD made in 
the United States is made but just a handful of chemists in california! Can 
you believe that? A half a dozen people make amost 100 million hits per year, 
and they have been doing it since the 1960s! This almost blows the mind! 

Forest Gump (Dec. 25, 1997 at 15:42):

Below are all the books that are in print that I know of which contain LSD 
synthesis procedures:

The Anarchist Cookbook, William Powell (1971);
The Book of Acid, Adam Gottlieb (1975);
Psychedelic Chemistry, Michael V. Smith (2nd Ed., 1981);
Recreational Drugs, Prof. Buzz (1989);
Practical LSD Manufacture, Uncle Fester (2nd Ed., 1997);
TIHKAL: The Continuation, Alexander Shulgin (1997).

So, which ones do I recomend for someone serious about LSD chemistry? Well, 
all of them! But not for the reasons you might think at first.

Most of these books contain serious errors. The Anarchist Cookbook for example 
has a method of "Making LSD in the kitchen" which is incorrect of course, 
although it does give an accurate procedure which is merely a reprint of the 
first part of Pioch's patent method. The Book of Acid calls to use sodium 
nitrate in one method, when in fact it is sodium nitrite which is used in that 
procedure. Recreational Drugs doesn't really contain anything that wasn't already 
in Psychedelic Chemistry, although it does give an incorrect LSD structure. All 
these books can go a long way in developing one's critical faculties though -- 
which is an important attribute for an LSD researcher to have, considering the 
B.S. factor that surrounds LSD.

So, which of these books do I think are the most important to have? 
All the books listed below, in order of importance:

1.) Psychedelic Chemistry; 2.) Practical LSD Manufacture; 
3.) TIHKAL.

Again, not for all the obvious reasons. Number 1 and 2 contain many journal 
references, and so can be a good step-off point to the real gold mine: the 
chemical journals at your nearest university science library. TIHKAL and #1 
both have the most up-to-date method, although that's the only method TIHKAL has.

Believe it or not, you can probably start learning about LSD chemistry right 
now if you have a chemistry text-book or are near any library. Just look-up the 
following (numbered in order of importance):

1.) carboxyl group;
2.) carboxylic acids;
3.) amides;
4.) amines;

also, look-up:

acid halides;
anhydrides;
mixed anhydrides;
hydrazides;
azides;
azoles;
esters;

and of course, alkaloids.

You see, LSD is an amide. LSD is usually made from lysergic acid which is a 
carboxylic acid and diethylamine which is an amine. Lysergic acid is in turn 
usually made by degradation of an amide, such as ergotamine.

All of these procedures involve the changing of one functional group: the 
carboxyl group. A good LSD chemistry researcher will devote much (MUCH) study 
to this group. 

I hope that this has been helpful.

-- Forest Gump 

--------------------------------------------------------------------------------
Forest Gump: 

CB: (2) Another dodgy thing about Fester's "Practical LSD Manufacture" is his 
recommendation to make LSAs by growing ergot on rye and to plant your own rye 
field in order to do this! Is the man mad? Fester appears to be ignorant of the 
existence of C. paspali.

FG: Yes, Fester is a bit loopy to think that prospective LSD chemists are going 
to become Farmer for a Year. Although the method certaintly works, the labor and 
amount of solvents required make it impractical for one or two people.

--------------------------------------------------------------------------------
some more references:
--------------------------------------------------------------------------------

CB: (4) In D. M. Perrine's book "The chemistry of mind-altering drugs" pages 
274-278 outline syntheses of LSD. He includes both modern total synthetic 
methods and clandestine methods [he figures that lysergic acid is made from 
either growing C. paspali to produce paspalic acid OR by diverting LSA from 
medicines]

Some of Perrine's references are:

Kornfeld et al; JACS 1956, 78, 3087-114 [early obsolete method]
Horwell; Tetrahedron 1980, 36, 3123-49 [review of early synth]
Oppolzer et al; Helv. Chim. Acta 1981, 64, 478-81 [modern total synth]
Oppolzer et al; Tetrahedron 1983, 39, 3695 [modern total synth]
Rebek & Tai; TL 24, 859-60 (1983), (and refs. therein.) 
	"A New Synthesis of Lysergic Acid", [total synth from tryptophan]
Rebek, Tai & Shue; JACS 106, 1813-19 (1984) 
	"Synthesis of Ergot Alkaloids from Tryptophan"
Kobel et al; Helv. Chim. Acta 1964, 47, 1052 [paspalic acid form C. paspali]
Troxler; Helv. Chim. Acta 1968, 51, 1372 
	[Isomerisation of paspalic acid to lysergic acid]

CB: (5) In M. V. Smith's "Psychedelic Chemistry" growth of C purpurea on 
synthetic media is described. Just about everyone claims that C purpurea will 
only grow on grain in a field. What's Up Doc?

FG: Getting species of Claviceps to grow in culture is easy. Getting species 
of Claviceps to grow in culture and produce lysergamides' is what's hard. 
I'm sure M. V. Smith's method in said book will work just fine for _growing_ 
Claviceps species, but it will all be for nought, as no lysergamides' will 
be produced by it.

Successful culture methods have been developed which use specific strains of 
both C. paspali and purpurea to produce as much as 2 to 5 g of lyseramides' 
per L of culture!!!! 

I direct you to "Biosynthesis of Ergot Alkaloids and Related Compounds", 
Tetrahedron, Vol. 32, pp. 873-912 (1976). On page 883 under the heading 
"Industrial production of ergolines" it gives a brief overview of what I 
just mentioned, and gives references to those procedures.

I hope that this has been helpful for you.

--------------------------------------------------------------------------------
Subject: References as promised...
From: aankrom@blackfoot.ucs.indiana.edu (aankrom)
Date: Thu, 7 Apr 1994 14:41:27 GMT

FN Johnson et al, JMC 16, 532 (1973) "Emetic Activity of Reduced Lysergamides", 
(LSAs using s-amine and POCl3) JACS 76. 5256: TL 1969, 1569.

Detlef Groger - Chapter 12 - Ergot, p 321
----------------
References:

Boisynthesis of ergot in submerged culture: Arcamone et al, 
1961, Proc. Roy. Soc. B155, 26.

Stoll & Hofmann - In "The Alkaloids" - ed Manske & Holmes, vol 8, 725-83.

Fetoclavine & fumigaclavine in Aspergillus fumigatus Fres, Spilsbury & Wilkinson 
1961, fumigaclavine in Rhizopus nigricans - Yamano et al, 1962, 

--------------------------------------------------------------------------------
KrZ - posted 06-21-98 06:57 PM CT (US) - Hive

http://www.alltheway.com/html/ergot.html

CA: 71:P69351y : describes mutants of strain NRRL 3027 producing 2270mg/l of 
ergoline compounds of which 85% were amides of lysergic and isolysergic acids. 
(Swiss patent application)

CA: 77:P156333n : describes a method used to get 9.75g pure lysergamides from a 
10 litre fermentation originally containing an estimated 15g.

CA: 94:13992r : reference Indian Drugs; 1980; 17(8) 228-31 (Eng.)
CA: 90:118108c : reference Indian Drugs; 1979; 16(4) 88-93 (Eng.)
Very interesting>:-||

CA: 102:219574y : Serbo-Croat areticle describing 2.2g/l 
prod. by C. paspali Stevens and Hall (1984).

Life History and Poisonous Properties of Claviceps paspali; 
H. B. Brown (Mississippi Agricultural Experiment Station); 
Journal of Agricultural Research ,vol. 7(9), pgs 401-405. 
describes on brief glance through it --- germination of the yellowish-grey 
sclerotia found on Paspalum dilatatum Poir. observed in the region of the 
Mississippi Agricultural College.
Also contains reference to Stevens and Halls' original article (1910).

* Biotechnological Exploitation of the Ergot Fungus (Claviceps Purpurea); 
Karl Esser and Andrea Duvell; Process Biochemistry, August 1984 pgs 142-149.
Synopsis: "The alkaloids of the ergot fungus C. purpurea and related species 
already known as drugs in the middle ages are still finding many uses in 
medical therapy (he he). Since the supply of natural grown ergots is not 
sufficient, the biotechnological production of ergot alkaloids has gained in 
importance. This requires not only an undestanding of physiological and 
environmental conditions, but also concerted breeding in order to increase 
and stabilize the production level."

* Biology of Claviceps; Willard A. Taber; Chapter 15 (sorry - i don't remember 
which book this came from, but it should be indexed under Taber in Biological 
Abstracts) pgs 449-486.
"If one desires isolates of C. paspali (which are high producers of simple 
amides), one must go to paspalum grass. ... C. paspali differs from all other 
species in possesing a yellowish tan cauliflower- shaped sclerotium rather 
than the purplish banana-shaped sclerotium, and it has been suggested that 
this species be trasnsferred to the genus Mothesia. "

*The Ergot Alkaloids; A. Stoll and A. Hofmann (THE); Chapter 21, The Alkaloids, 
Manske (ed. ?) vol. VIII, pgs 725-779+.
Describes lots and lots and lots of chemical detail regarding everything from 
biogenesis to complete chemical synthesis as a means of confirming structure. 
Also has a section completely devoted to "Derivatives of Ergot Alkaloids" in 
which the following processes for synthesizing amides are discussed:

=> The azide process.
=> DMF-SO3 mixed anhydride method.
=> mixed Lysergic acid trifluoroacetic anhydride.
=> Lysergic acid chloride hydrochloride method.
=> N,N'- carbonyldiimidazole as condensing agent (Best IMHO).

Kobel, Schreier, Rutschmann. Helv. Chim. Acta 1964, 47, 1052


--------------------------------------------------------------------------------



