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                  TMA-2 from Sweet Flag Root (Acorus Calamus)
                By Randolph Carter - The Perennial Dream Questor
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Sweet flag grows throughout most of north amerika east of the rockies in the
wild state in wet areas where wild rice and reeds would feel at home. I found
immense stands in Tennessee and northern Mississippi.Therefore my granola-head
sensibilities were not offended by the copious gathering, for extraction and
transplanting of this aquatic plant to the wilds of extreme north Georgia.
It's most prevalent constituents are asarone, eugenol and esters of acetic and
heptic acids. Even though this treatise includes my full dreams from the plant
roots, I would be remiss if I did not point out that calamus oil is readily
available from most of the usual suspects who deal in essential oils. I have
found that this is a MUCH more attractive from scratch type of synthesis than
sassafras / safrole ever dreamt of being. That is my impetus for doing this
research, to wit what can I use that is VERY prevalent in my area to produce a
most dreamy not-drug. My experiences with the results of this procedure have
been VERY favorable received in most tests (which have been VERY extensive).
Field testing indicates that dosages in the 25 to 50 mg range result in some
VERY fine psychedelic dreams that are quite facilitative to sexually enjoyment
with single or multiple sexual partners unlike many heavy psychedelics.

Anyways here is the rest of the story as paul harvey sez...


Steam Extraction Technique
--------------------------
The extractor is about 2' in height and about 16" in diameter made of stainless
steel and has tight fitting "connections".Imagine a large pot with a drain
spigot on the bottom, on top of the pot is an approx 1 1/2 gal "steamer" with
sealing lid and a bottom of preforated holes. (i lined the bottom of this with
fine gauge stainless steel screen finer than pipe screens..from industrial
sources to minimize grit and small pieces of root fibers...) To operate i
dreamed that i charged the "basket" with all the ground roots (ground by a small
hammer mill used on the farm for other herbs we sell...chopped root would work
equally well we feel...)the top was sealed on with silicone stopcock/joint
grease and it was heated to boiling and maintained there for about 6 hours per
load (7 loads required for 10 kg...). After cooling down the top is removed and
the water with an oil layer was drained into a nalgene carboy with spigot which
allowed for a "crude" seperation of the oil and a small amount of water. Then it
was shook in the carboy with the applicable washes mentioned below before being
put in a "real" 2l sep funnel for final seperation.


Calamus Essential Oil
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Approximately 10 kg of dried calamus root were steam distilled with the help of
the above mentioned stainless steel juicer/extractor obtained through cumberland
general store. (This item is commonly found in seed catalogs from several
companies as well). This yielded 330 g of viscid light yellow oil with a bitter
taste, which was only slightly soluble in water. After separating the oil, the
oil was washed with first a water solution of sodium carbonate then water then
it was seperated from the water layer then dried over drierite overnight before
further usage.

Yield = about 320 g clean calamus oil.


Asarone
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Next this oil was fractionally distilled to yield a fraction at 185 to 200 c
which was chiefly asarone.

Yield = about 210g


2,4,5-Trimethoxyphenyl-2-nitropropene
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100g asarone in 1 l ether was placed in a 3 l rb flask with a saturated solution
of 500g sodium nitrite in water and setup on a mag stirrer. A pressure equalized
addition funnel which was filled with 800ml of 25% sulfuric acid was then
affixed to the flask and dripped into the solution over a period of 5 hours with
magnetic stirring. After the 5 hours it was allowed to sit over night (about 14
hours...). In the morning the solution was filtered then the filter cake was
washed with water then ethanol then ether. The resulting cake of crystals was
dissolved in 500 ml ethanol with 50 g sodium carbonate in it with mag stirring
and gentle heat (below 30 c). Once it was completely dissolved it was allowed to
cool 1 hour then 1.5kg of ice was added then adding 1l dilute hydrochloric acid
acidified it. It was allowed to sit about 1 hour at 0c then filtered and washed
with water and then let dry. This yielded 1/2 cm yellow needle crystals of the
2,4,5 substituted nitropropene with a mp of 100c.

Yield = about 78 g


2,4,5-Trimethoxyphenyl-2-propanone
----------------------------------
75 g of this nitropropene were placed in a rb flask rigged for reflux and
addition funnel via claisen adapter with 60g iron filings and 1.2g ferric
chloride in 100ml toluene. This solution was brought to reflux then 110g
concentrated hydrochloric acid were dripped in over the course of 4 hours.
Continue reflux for an additional hour after addition is complete then let cool
to room temperature. Solution was then flushed with 2l water and subsequently
extracted four times with 200ml ether. The ether extract was dried overnight
over drierite filtered then the majority of the ether was distilled off before
vacuum drying the ketone.

Yield = about 40g


2,4,5-Trimethoxyphenyl-2-aminopropane Hydrochloride (TMA-2 HCl)
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40g ketone was placed in a rb flask setup for simple distillation with 35 ml
formamide 4ml 90% formic acid (adjust as necessary to achieve 4.5 ph) and slowly
brought up to about 140 c over 4 hours. (This is interactive at this point. what
you are looking for is a few small streams of bubbles, kind of like a coke
fizzing when about half flat...). Keep the temperature as low as the reaction
will allow and raise the temperature only when necessary to keep reaction going.
Check the ph about every 4 hours and add formic as necessary to keep ph about
4.5 after 28 hours the reaction temperature had reached the ceiling temperature
of 180 c (about 25 ml water had distilled over by this point...). The solution
was allowed to cool for 2 hours then extracted four times with 100ml benzene or
toluene, then the benzene/toluene was distilled off and the solution is put in
a rb rigged for reflux 35 ml concentrated hydrochloric acid is added and it is
refluxed for 8 hours. The solution is then cooled for 1 hour and then chilled
to 15c basified with 10% sodium hydroxide and extracted four times with 100ml
ether. This extract was dried overnight over drierite and filtered in the
morning before vacuum evaporating the amine oil. The oil was gassed in the
normal manner to yield fine white crystals with an mp of 189c.

Yield = 36.5g of high energy FUN! [ TMA-2 Hydrochloride ]

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