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DMT Synthesis

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blackclo

Rising Star
OG Pioneer
Found this DMT synthesis from the Rhodium site. Me, having absolutley no chemistry knowledge can't really grasp it but I'm sure that there are some Chem students and such that can prob glean something from it. It looks considerably more difficult than extracting from plant sources but I thought I'd add it for novelty's sake 😉 [color=red:bea4242e47]DMT Synthesis[/color:bea4242e47] [color=violet:bea4242e47]Step I[/color:bea4242e47] 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. [color=violet:bea4242e47]Step II[/color:bea4242e47] 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 0C 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. [color=violet:bea4242e47]Step III[/color:bea4242e47] 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.]
 
I always wonder with this kind of chemical experimenting: How big is the change of you accidently creating a deadly or seriously toxic potion? In the end you need to have a good proofing tool to check if it's good DMT you've just created and preferably, that shouldn't be you.
 
I thought about it and I think your right Traveler. This synthesis should only be tried by someone very knowledgable in this field and who knows what their doing. I prob should delete this topic as the risks are too great in someone doing something wrong. Also I see that the synthesis should have diagrams to go along with it but there were none to download making it more difficult. So yeah, if you really really know your stuff it's worth a look at this but otherwise I'd take Travellers advice and stick to plant extractions as their SO much easier.
 
Well, I think it's a good thing to leave this knowledge here but just make sure that if you are experimenting you've got some tool (spectograph?) to identify the purity of the DMT and make sure you don't get any harmfull other substance beside it.
 
hi, according to nick sands dmt produced via the oxalyl chloride method is typically purified by vacuum distillation. it is then crystallized by dissolving 1 part dmt in 2 parts ether, adding this to 8 parts hexane, and cooling. the identity of the product can be verified well enough by taking it's melting point. according to rumor the tryptamine + CH3O + cyanoborohydride method in contrast requires chromatography to satisfactorily purify the product. this synth is even more difficult using ordinary borohydride, which requires simultaneous proportional addition of reagents if it is to work at all. shulgin's tryptamine + MeI, followed by dequaternization method is more facile but relatively low yielding. swim speculates one might make MeBr from NaBr + MeOH + H2SO4 and lead the gas into the tryptamine reaction. MeBr and MeI are dangerous poisons of course. the russian tryptophol + dimethylamine + nickel catalyst procedure is reported to give 93% yield in 4 hours with no hydrogen gas or pressure required. as far as i know no one since the origional authors has performed it. tryptohpol can be produce via erlich method using yeast and tryptophan (details on request). or via LAH or Na reduction of esther of indole-3-acetic acid. first one to accomplish this with an aluminum amalgam reaction wins the son of shulgin award...
 
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