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This is from _The Psychedelic Guide to the Preparation of the
Eucharist, in a few of its many guises_, as edited by Robert
E. Brown and associates of the Neo_American Church League for
Spiritual Development & the Ultimate Authority of the Clear
Light (1968), 2nd edition (1971)
DMT Synthesis
STEP I
Using an area of good ventilation or a fume hood, place a
1000 ml two hole roundbottom flask in an ice bath using the
setup in Figure II (you want a wobble stirrer in the top hole
of the flask, and a separatory dropping funnel into the side
entry). Add 400 ml cold anhydrous ether to the flask, in which
60 g indole is then dissolved, using the stirrer. To 100 ml
anhydrous ether in a separatory funnel add 50 g oxalyl
chloride. Slowly drip this solution into the vigorously
stirred indole solution over a period of 10 to 15 minutes.
Continue stirring 10 minutes longer. Allow the precipitate to
settle a few minutes and decant the liquid. Add anhydrous
ether and mix well. When satisfied as to the purity of the
precipitate, leave the golden precipitate in the flask for the
next step, which must follow immediately. Yield is
approximately 100 g.
STEP II
Dimethylamine reacts readily with indole oxalyl chloride.
Use about 400 ml ice cold anhydrous ether in the same 2 neck
1000 ml RB flask used in Step I, with the precipitate in it
from Step I. Cool the ice bath further by using salt and ice.
Estimate the weight of the precipitate and use 100 g indole
oxalyl chloride. For this weight of IOC use two entire 50 g
containers of diethylamine since it will not keep if the
container seal is broken. Cool the amine in container much
below 0 C and dissolve 1 part amine in 3 parts anhydrous cold
ether. Amine may be stored in this solution. For use, warm
stock solution to room temperature and use the appropriate
aliquot. Set up the entire apparatus the same as when adding
the oxalyl chloride. Add the amine solution slowly to the IOC
with vigorous stirring. Stir for 1/2 hour after the addition
is complete. Vacuum filter the precipitate, using ether as a
wash. It is better to slurry the ether water with the
precipitate before filtering [method used]. Recrystallise from
hot ethanol or from a 50-50 methanol-benzene mixture.
STEP III
Prepare apparatus as in Figure II (1-hole 1000 ml RB
flask set in heating mantle on magnetic stirrer with stir bar
in flask, and condenser inserted into top of flask). Prepare
the indole glyoxyl amide by melting and casting into sticks if
ether is to be used as a solvent. Aluminium foil makes a good
mould for casting pieces that will fit through the condenser.
Also a Soxhlet extractor may be used to add the crystals by
slow solution into the ether. Tetrahydrofluran, if available,
dissolves IGA and the compound is added slowly in the solution
form [method used].
To a stirred mixture of 15 g LiAlH4 in 100 ml anhydrous
ether (or THF [used]) slowly add the sticks (or solution
[used]) of IGA until 20 g have been added. Keep the rate of
reaction at a reasonable rate or boil-over may occur [do
say!]. Stir and reflux for 90 minutes after the addition is
complete. Cool in an ice bath and begin to cautiously [do
say!] hydrolyse with chips of ice or a cold solution of
methanol, added through the condenser. When there is no
further reaction, add a few ml extra water and allow to settle
finally and decant the clear liquid into an evaporating
vessel. Filter the residue and wash several times with
ether-methanol or THF-methanol [used]. Evaporate the combined
extracts and if necessary, seed the heavy syrup with crystals
of DMT. With no seed crystals the product may take days or
even weeks to crystallise [weeks]. This crude product is
adequate for smoking [do say!]. In order to purify DMT, begin
after the LiAlH4 has been hydrolysed with methanol. Add 500 ml
satd. Na2SO4 solution, mix and filter. Wash with ether or THF
and neutralise the filtrate with 0.1 N HCl. Extract with ether
in a separatory funnel and neutralise the lower layer with 0.1
N NaOh, extracting this solution in turn with chloroform. The
chloroform layer is dried over anhydrous Na2SO4, concentrated,
and from it DMT crystallises on addition of petroleum ether.
The mother liquor can be chromatographed on an alumina column
using benzene-methanol in a 99.8 to 0.2 ratio. [This last
purification is quite difficult.]
--
John Collier Email: jcollier@ariel.ucs.unimelb.edu.au
HPS -- U. of Melbourne Fax: 61+3 344 7959
Parkville, Victoria, AUSTRALIA 3052
=============================================================================
DET Synthesis (Diethyltryptamine)
STEP I
Same as for DMT
STEP II
Use 200g diethylamine per 100g IOC. Diethylamine is less volatile and
poisonous than dimethylamine, so cooling is not necessary, but the fumes are
poisonous. Use the same procedure otherwise. Diethyl derivative is easier to
work with.
STEP III
Use same procedure and equipment. Use 22g indoleglycoxal diethylamide. The
final product is also easier to purify.
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NOTES
STEP I
Absolutely anhydrous ether is essential. A container that has been opened
previously is no longer anhydrous. Where cooled reactions are necessary,
remember that moisture is drawn to cold objects, and cold reagents, when left
open or poured, become quite wet. This applies to the initial reaction on all
three steps. A magnetic stirrer will not work for steps I and II. The
vigorous wobble-stirrer has been found adequate do deliver the violent
stirring needed, especially when several stirring balls are used in
conjunction with the paddle-bar. Sparkless motors must be used around ether.
Oxalyl chloride is very toxic and ventilation or a fume hood must be used.
Water vapor hydrolyses product I, producing a gummy dark-red mass. Proceed
to Step II as soon as possible.
STEP II
Refer to notes on anhydrous ether, stirrer, sparkless equipment, and
ventilation in the notes for Step I.
The color of the precipitate lightens somewhat as the amine is added to the
compound I.
The water in the ether is used to dissolve all low-molecular-weight amines.
STEP III
The crystalline amide is difficult to add to the LiAlH4 mixture. A Soxhlet
extractor may be used to add the amide by placing it in-between the flask and
condenser. Casting it into rods or bars is one of the simplest methods.
Tetrahydrofuran, if available, enables the indole glycoxal amide to be
dissolved and added as a solution; a procedure which is best and fastest of
all. LiAlH4 is a very dangerous inflammable compound, especially so when in
ether solution. The ether must be absolutely anhydrous or a violent
effervescence occurs, destroying the LiAlH4 and creating a fire hazard.
Contact of LiAlH4-ether solution with any water, damp materials, or even
chemically bound water such as cellulose causes spontaneous combustion. A
safety shield made from auto windshield material is a must when working with
LiAlH4 in any form. Handling LiAlH4 is done wearing rubber gloves in a dry or
inert atmosphere with a minimum of friction involved. Hydrolysis of the
complex is dangerous and should be done slowly and cautiously, using an
ice-bath to cool the mixture.
Difficulty in producing crystals the first time should cause no concern
since many organics need seed crystals to crystallize. The syrup may be used
for some purposes but be sure to save some seed crystals if you should happen
to get some.
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BIBLIOGRAPHY
Journal of Organic Chemistry Vol.23, p.1977
Journal of American Chemical Society Vol.76 p.6208
Journal of American Chemical Society Vol.82 p.2184
Chemical Abstracts Vol.53, p.11324
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A FINAL NOTE
(added Mon Apr 24 21:21:25 PDT 1995 -- Yogi S*/Lamont G)
The DMT recipe is misleading. Dimethylamine is a gas. DEA & DPA
are liquids. DMA is typically sold as 40% solution dissolved in
water. Since the indolyl reaction *must* be anhydrous, you will
get absolutely *nothing* if you use the 40% solution. You'd either
have to extract it into ether, and dry the ether. Or use the dry
gas directly.