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