Newsgroups: alt.drugs.chemistry,alt.drugs,alt.psychoactives
From: ez026264@dale.ucdavis.edu (Speed Raver)
Subject: d-meth synthesis
Message-ID: <Cu2397.F53@ucdavis.edu>
Date: Fri, 5 Aug 1994 09:48:43 GMT

Sorry if some of the spelling looks tweaky. My C key is acting really 
weird. Also, there are diagrams at the end for reference.

SYNTHESES THAT SUCK:

There've been a lot of synthesis methods proposed on UseNet for 
synthesizing methamphetamine. Thus far, I haven't seen one that I imagine 
would work.

One, from Phrack magazine, is the "tried and true method" for prepping
meth from Vick's nasal inhalers. Vick's nasal inhalers contain
"l-desoxyephedrine," another name for "l-methamphetamine." The l- isomer
of methamphetamine is the relatively inactive one, usable as a (mild)
nasal decongestant. The d- isomer is the one that everyone wants and that 
Uncle Sam has declared is just too cool for anyone except doctors.

The procedure described would extract the l-meth froom the inhalers and 
collect it and that's  it.  I'm sorry, but the Isomer Fairy can't wave 
her magick wand and reverse the chirality of the molecule. The only way 
to change between the two isomers is to oxidize the l-meth into 
phenylacetone, condense it with methylamine, then reduce it. Sorry, but 
soaking inhalers in HCl then separating the "juice" with Et2OH just won't 
do it. You'll get l-meth and that's that.


A more credible souding one mentions that "methamphetamine is prepared by 
the calalytic reduction of pseudoephedrine in acetic acid" blahblahblah and 
then goes on to describe, not catalytic reduction via acetic acid, but 
reduction with sodium borohydride. I'm sorry to say that no method 
attempting to directly reduce (pseudo)ephedrine's hydroxyl group is going 
to work. You can't expose it to a strong acid, or a weak acid, or sodium 
borohydride, or even lithium aluminum hydride and expect it to reduce at 
all. As with the Vick's Inhalers "recipe," you get a lot of SOMETHING, 
but it ain't d-meth. All you'll be left with is your (pseudo)ephedrine 
and a bunch of acid, lithium, and/or sodium and lotsa hydrogen gas. This 
is because the hydroxyl group (the OH in ephedrine) is on a very acidic 
carbon (the first carbon away from the ring) and a hydroxyl group is very 
basic. If the hydroxyl were on the second carbon from the ring (the 
carbon with the amine group, the NH2 or NHCH3), there might be some 
chance, but it's not and there's not. You're not getting a basic group 
off an acidic carbon without a fight, and acids, borohydride, and 
LiAlhydride aren't gonna fight that hard.


SYNTHESES THAT DON'T SUCK:

One of the easiest ways to make methamphetamine is from amphetamine. Of 
course, this assumes you have amphetamine in the first place, but let's 
just pretend you have some and you want to spice it up a bit.
The difference between amphetamine and methamphetamine is the addition of 
a single methyl group (CH3) to the amino group sticking off the middle 
carbon atom in the chain. Fortunately, substituting amines is really 
simple. Vaporize your amine (your amphetamine) with a bunch of vaporized 
chloromethane (CH3Cl, a solvent) and some gaseous pyridine...
voila, the amino group takes the methyl from the chloromethane and lets a 
hydrogen go. The hydrogen joins the liberated chlorine, and the resulting 
HCl is soaked up by the pyridine. The pyridine is optional. Adding it 
drives the reaction a bit by pulling the excess HCl out of the equation, 
but it's not neessary.


Assuming you don't have amphetamine lying around, an easy synthesis with 
a very high yield is to reduce the condensation product of phenylacetone 
and methylamine. The benefit of this method is that different amines can 
be used to produce novel N-alkyl amphetamines (ethamphetamine, 
tert-butylamphetamine, etc)


Making it from ephedrine or pseudoephedrine is possible. The only 
difference between methamphetamine and (pseudo)ephedrine is that damn 
alpha-hydroxy group. Reacting your ephedrine with thionyl chloride 
replaes the OH with Cl to produce N-methyl-alpha-chloroamphetamine as an 
intermediate. Hydrogenating this product is easy: use lithium aluminum 
hydride, sodium borohydride, or even hydrogen gas with nickel or platinum 
metal as a catalyst. The product of this step is N-methylamphetamine and 
HCl. Evaporate off the water and you have methamphetamine hydrochloride.


A surprisingly simple synthesis is possible from the amino acid
phenylalanine, which is available at health food stores for about $14 for
100 tablets. Phenylalanine is 2-amino-3-phenylpropanoic acid, which is
more or less amphetamine with a COOH where the CH3 should be at the end of
the chain. Thionyl chloride will replace the OH with a Cl, which falls off
and is replaced by H when you give it lithium aluminum hydride, sodium
borohydride, or hydrogen gas and nickel/platinum. If you use hydrogen and
metal for that step, you'll have to reduce the carbonyl group with one of
the hydrides, so best save time + effort and use them and do both
reductions at once. When that carbonyl is reduced, you now have
amphetamine. Go back up to that first one I mentioned for upgrading
amphetamine into methamphetamine. 


Note that azll of these (and probably anything anyone ever comes up with) 
will give you a mix of d- and l- isomers. The d- is cool, the l- is shit, 
remember. If you have time, energy, and equipment, you can separate the 
two and reprocess the l- into d- by oxidizing it and re-aminating it as 
described in the "critique" of the Phrack synthesis.


DIAGRAMS:

                    H
    /\\     / \     NH
  /    \\ /     \ /
 ||      |       |
 ||      |       |
 ||      |       CH3               amphetamine
  \    //
    \//
                    H
    /\\     / \     NCH3
  /    \\ /     \ /
 ||      |       |
 ||      |       |
 ||      |       CH3               methamphetamine
  \    //               has a CH3 at N that amphetamine doesn't
    \//

             OH
             |      H
    /\\     / \     NCH3
  /    \\ /     \ /
 ||      |       |
 ||      |       |         ephedrine and pseudoephedrine
 ||      |       CH3      the difference is whether the OH
  \    //                        points up or down
    \//

                    H
    /\\     / \     NH
  /    \\ /     \ /
 ||      |       |
 ||      |       |
 ||      |       C=O              phenylalanine
  \    //        |            compare to amphetamine
    \//          OH



Article 94300 of alt.drugs:
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From: yshan@bcarh697.bnr.ca (Yogi Shan)
Newsgroups: alt.drugs.chemistry,alt.drugs,alt.psychoactives
Subject: Re: d-meth synthesis
Date: 5 Aug 1994 21:43:01 GMT
Organization: Bell-Northern Research, Ottawa, Canada
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ez026264@dale.ucdavis.edu (Speed Raver) wrote:

**>  I'm sorry to say that no method attempting to 
**>  directly reduce (pseudo)ephedrine's hydroxyl 
**>  group is going to work.

Your post was interesting, but this is not quite true.
Direct hydrogenation over Pd or Pd on a carrier is well
known and facile.  You add a little perchloric, 
phosphoric or sulphuric acid, which esterifies the-OH 
group that you're complaining about.

Thus making the intermediate halide via SOCl2, like
you mentioned, is unecessary.

**>  Note that all of these (and probably anything 
**>  anyone ever comes up with) will give you a mix 
**>  of d- and l- isomers.

Hydrogenation starting with (-) ephedrine, whether
direct or via the halide, will give d-meth.  If
you start with dl-ephedrine, you get dl-meth.


Yogi


From: dcopela@mail.pacifier.com (David Copeland)
Subject: correct ways to manufacture methamphetamine
Date: Tue, 16 Dec 1997 00:00:00 GMT
Message-ID: <34963053.0@news.pacifier.com>
Organization: Pacifier Internet Server (360) 693-0325
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Reply-To: dcopela@pacifier.com
Newsgroups: alt.drugs.chemistry



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 This information is for information purposes only. Any attempt to put 
this into practice can (and probably will) result in long prison terms. It 
is with much intrepredation that I write this. Methamphetamine wreaks much 
havoc in society. However knowledge should never be wasted.

        There are two common ways to make meth. One is with d-ephedrine or 
pseudo ephedrine. The other is with phenyl-2-propanone. The difference is 
that with ephedrine you get the d-isomer only while with p-2-p you get a 
mixture of both isomers. There is some discussion as to which is better 
but most "experts" prefer the p-2-p product. 

Okay. 

1: ephedrine method. In a round bottom flask place 1000gms of ephedrine, 
250 gms of red phosporus,1000ml of hydriotic acid and 1 oz of 
thiosodiumsulfate. Place a condenser on top of the flask and reflux the 
mixture for 48 hrs at 120 degrees C. Cool the mixture. Add a 10% solution 
of sodium hydroxide slowly since heat will be evolved until the Ph of the 
mixture is 14. You should have an upper and lower layer. Separate the 
upper(oil) layer from the lower (water) layer. Distill the oil layer 
(steam distillation is the best-go look it up). Mix the distillation 
product with a 10% hydrochloric acid solution until the Ph of the mixture 
is 8.0. Evaporate the water (steam bath) and the final product will 
crystallize.

2: p-2-p method. In a round bottom flask of suitable size place 400ml of 
p-2-p, 2000ml of ethyl alcohol (everclear works fine), 400 gms of aluminum 
(reynolds wrap or better yet 1100 grade aluminum foil or shavings) and 
2000ml of 30% (not 40%) methylamine. Add 1/3 gram of mercuric chloride and 
quickly fit the flask vertically with the biggest condenser you have. The 
reaction should get warm. If not heat it a little until it does. This 
reaction is VERY exothermic (gives off heat). As soon as the mixture 
starts to bubble and get warm get ready to put the flask in an ice bath to 
keep it under control. Let the reaction run its course until it starts to 
cool then heat it for another hour or so. Cool the reaction, filter the 
mixture with a buchner funnel under vacuum to remove the solid by-product. 
Place the clear filtered liquid in a flask set up for distillation and 
distill off the alcohol (under vacuum preferably). You will know when the 
alcohol is gone when the mixture becomes cloudy. Let the mixture sit and 
it will separate into two layers. The bottom layer is water (etc) and the 
top layer is Methamphetamine. Separate the top layer in a separatory 
funnel and (steam distill it first for the best results) mix it with 10% 
hydrochloric acid until the Ph of the mixture is 8.0. Evaporate the 
mixture on a steam bath ( Or a  pyrex plate placed on top of a pot of 
boiling water) and it will crystallize into the final product. 

The whole key here is the purity of your starting ingredients. Pure 
material equals a pure product.

Again this is for information only. To put this into practice is illegal 
and can result in fines and/or imprisonment.

ephedrine is impractical to make. p-2-p can be made in many ways. It is 
NOT available otherwise . It can be made by reacting phenylacetic acid and 
lead acetate. Or better yet phenylacetic acid, acetic anhydride and sodium 
acetate. There are many other ways to make p-2-p (Thorium catalyst 
reduction of phenylacetic and acetic acids, The Bader and Nightingale 
aceto aceto nitrile reaction etc. Go to a college library.

   

From: mark.pawelek@virgin.net (Mark Pawelek)
Subject: Re: methylamine and methylamine hcl
Date: Tue, 19 Aug 1997 00:00:00 GMT
Message-ID: <33f9f22e.20385994@news.virgin.net>
References: <5smj7c$6qn@basement.replay.com>
Organization: Virgin Net Usenet Service 
Newsgroups: alt.drugs.chemistry


On 11 Aug 1997 10:41:16 +0200, nobody@REPLAY.COM (Anonymous) wrote:

>1. Theoretically if one can to consense the product of methylamine and 
>phenylacetone into methamphetamine (rather simple really) then what 
>happens if you substitute methylamine.hcl in the reaction.  Does the hcl 
>interfere with the rection?? If it makes methAmphetamine.hcl then this 
>would take ALOT of heat to boil before re-condensing? IS this in-fact 
>what happens?  Or does it just screw things up..
>

From what I know the reaction still works with meth HCl. You can read
this up in the Chemical literature - it's been known about for well
over 60 years.

>2. If you wanted to change methylamine.hcl into methylamine, you could 
>disolve in water, make it basic with NaOH then what do you extract 
>with??

Yes.  But MeNH2 is very soluble in water. 1 part of water dissolves
1000 parts of MeNH2.  It is not at all soluble in organic solvents.  

>Chem references (online) are VERY short on detail when it comes 
>to agents that methylamine is solutable in.

Look it up in a book - The Merck index should be available in your
local library.  If you post obviously silly questions like this people
will think that you are lazy or incompentant or both.  They will not
want to encourage your dependency on them by giving you answers that
you can find out for yourself.  Nevertheless I'll tell you - just this
once.

MeNH2 is not very soluble in orgainic solvents. eg. The solubility is
only 10% in benzene.

It is soluble in water and ethanol.

It is not soluble in CHCl3, acetone, ether or ethyl acetate.

You would not try to extract into an organic solvent as it wouldn't
work.

You could add base, increase the temperature and boil the MeNH2 off,
collecting the gas produced.

>
>3.  (Ok I lied there are 3 questions, so sue me)
>I have seen 2 synthetic routes for P2P however both involve shall we say 
>difficult to obtain precursors.  Are there any other synthetic routes??
>

Yes. There are loads of possible routes.  A good place to start is
"Advanced Organic Chemistry" by Jerry March. This inexpensive book
will keep you busy in the library for years - looking up the
references.  The simplest route to ketones is via the corresponding
alcohol and the corresponding alcohol is often easy to make and,
unlike P2P it is probably legal to possess!

There appear to be another 100 routes to ketones mentioned.  P2P is an
easy ketone to make because it has only one functional group.

Of course, I couldn't think of any reason why you would want to make
P2P.  Why not go straight to the chemical you really want by
condensing the imine [produced from MeNH2 and acetaldehyde] with
Benzyl Magnesium Halide in a Grignard reaction?

No, I won't give you the literature reference to this reaction.  It is
obsure and you will need to search hard to find it.  Clue. The time
was between 1945 and 1955.

>4. (Ok I lied again there are 4 questions.. really this is the last one)

I never trust people who lie to me!  Give up this bad habit unless
you're realy desperate and you can't avoid it.  I'm not moralising
here - I'm just telling you that people don't do favours for people
they don't trust.

>Has anyone any thoughts on the reduction of (pseudo)ephedrine via either 
>iodine/phosphorous (red) or HI/phosphorous.  I assume it racemizes the 
>product. Is this a correct assumption??  Also dies HI warrant the effort 
>or can Iodine/phosphorous be used instead, Does the additon of HI 
>significantly inprove the yield??

Yes, It's very messy.  I suspect that it might be easier to reduce the
ketone than it is the alcohol.

The Clemmensen reduction of aliphatic ketones to hydrocarbons uses
amalgamated zinc and concentrated HCl. The 3rd edition of Vogel's
Practical Organic Chemistry gives details of this. [but not for the
compound you want. Although there's no reason why it shouldn't work]
It too is a messy reaction [and that's why it is no longer used] but
the reagents are much more easily available.
>
>elusius and steve quest your comments would be grately appreciated..
>
My comments are: if you're going to mess about with HI or red P then
you should be studying at a university.

