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Another Stab at Salt

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Noman

Noman

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I was torturing myself by rereading Quantum Tantra's tek and came across a snippet of information that might be useful if true: " All DMT salts are insoluble in non-polar solvents -- with the exception of DMT acetate -- which is soluble in chlorinated non-polar solvents such as chloroform and DCM. Thus if you are using white vinegar (acetic acid) as your acid, you will need to use naptha or ether to defat as chloroform or DCM would extract the DMT acetate along with the oils and fats, defeating the purpose of this step." This would mean that one could extract MHRB with vinegar, defat with naptha, and then extract DMT acetate with DCM and evap. I dont know if DMT acetate is a nice dry snortable powder, but it seems worth a go if one could get some pure DCM or chloroform.
 
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Noman, i'm not sure that would work.. You already have your dmt acetate happily dissolved in distilled water; how can you ensure that by adding DCM or chloroform, the DMT acetate will actually migrate to those layers away from the distilled water? plus, you'd need to check that DCM and chloroform don't actually mix with the water (in the past i added two things, (maybe acetone and naptha, but can't remember for sure) and they didn't actually form layers! they just mixed in together) how about get a 250mL drinking glass, put an amount of DMT freebase powder in it (say 1 gram) and cover with around 20mL of distilled water (i'm guessing the dmt base will stay undissolved). Then add dropwise some acetic acid or tartaric acid and stir. add another drop, stir, etc.. until all your freebase has disappeared, and then evaporate in an oven under low heat like 90 degrees celsius.. ? hopefully DMT acetate and DMT tartrate have significantly higher melting points..
 
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According to Trouts Notes #FS-X4: 'Acetic acid should not be used in combination with chloroform during defatting(probablyalso true of methylene chloride).While it will work, DMT acetate is [i:55912f37e4]somewhat[/i:55912f37e4] soluble in chloroform and will be at least [i:55912f37e4]partially[/i:55912f37e4] extracted into it during defatting.' (My italics)
 
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I think it should work, but remember it's all dependent on the melting points of the salt. Ideally, with a MP of around 150 degrees you could no worries evaporate the water at 80-90 degrees (celcius), but if the MP of the salt is much lower then you'll likely evaporate that too Tihkal mentions: [quote:0696cda0f9="Tihkal: DMT"]As to salts, this last recipe above, taken from the literature, is the only claim of a valid hydrochloride salt of DMT [i:0696cda0f9]mp of 165-167 °C[/i:0696cda0f9]. In the original synthesis, by Manske, the following description appears. "The hydrochloride could be obtained only as a pale yellow resin which, when dried in a vacuum desiccator over potassium hydroxide, became porous and brittle." I have found no attempts at its synthesis in the literature, and I have personally had no success at all. The [b:0696cda0f9]picrate salt[/b:0696cda0f9] is well defined, used mostly for isolation and purification. [b:0696cda0f9]The oxalate is used occasionally in animal studies.[/b:0696cda0f9] Early human studies involving the injection of solutions of the hydrochloride apparently made by dissolving DMT base in dilute aqueous HCl, and neutralizing this with base to achieve an end pH of appropriate 6. [b:0696cda0f9]The fumarate is the salt specifically approved by the FDA for human studies, and this was the form used for human intravenous injection employed in the recent New Mexico studies.[/b:0696cda0f9][/quote:0696cda0f9] It's surprising that shulgin could successfully crystallise the hydrochloride; as he mentioned this is the only literature documenting successful crystallisation of DMT.HCl. Eitherway, i'd suggest a different type Don't think about picrate, apparently it's highly explosive (working with picric acid) Seems to be that the fumurate would have the most stable properties if that is the one being used by the FDA. Now how to obtain fumaric acid? i put this question on the nook so you can watch for replies if you like: Contact Support actually the more i think about it i'd 100% definitely be going for the fumarate.. --actually, after looking around it seems fumaric acid is inexpensive and used frequently in the food industry. I found a local supplier that has this although i don't know how dodgy it'd be to get it.
 
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back to tartaric acid giving dmt tartrate fumaric acid is insoluble in water which would make the proposed method tricky if it worked at all. apparently fumaric, maleic, and tartaric acid are all quite similar (not sure why). Maleic is relatively unstable and has a lower MP than both tartaric and fumaric acid. So possibly tartaric acid would be the best option. here's google info on those: Maleic acid - Wikipedia Fumaric acid - Wikipedia Tartaric acid - Wikipedia
 
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I guess I'm naive but why couldn't you just add the freebase to an excess of acetic acid? Wouldn't that convert it to the salt, and you could then just evaporate off the liquid? oops thats what Coschi said :)
 
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SWIM put 0.3g of dmt into 100ml water. Added hcl untill dissolved. Put in Oven at 50 Degree Celcius. When water had evaped. Thin film was left. Smell not like regular dmt but similar. Scraped and smeared. Would not crystalise. The color was transparent with a tint of blue/black. Think hcl is not the right acid for this. Or something else has to be done with it laiter.
 
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[quote:a87ffb2ab8="monkeyboy"]ummm.... it can be a real bitch to separate DCM and water.... At least thats what SWIM remembers from the old days when he used to play around with other things.[/quote:a87ffb2ab8] SWIM have been playing around with phalaris and used HPLC grade DCM for defat and extract. And DCM is not hard to seperate from acid or base water. Exept from that is sinks rather than float.
 
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It is documented almost everywhere that the hydrochloride salt of dmt will not crystallise acetate should work, but in all literature i see fumarate and oxalate and things like that. The fumarate is the one approved for human studies so i'd likely go for that or something similar (maleic or tartaric) the only problem with adding dmt base to excess dilute acetic acid (or any other) is that there will be excess acidic ions floating around which may not be the best if your idea is to inject them (although it may not matter a whole lot) - also when you evaporate your liquid you'll be left with the excess stuff as contaminant
 
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[quote:45a911adb3]the only problem with adding dmt base to excess dilute acetic acid (or any other) is that there will be excess acidic ions floating around which may not be the best if your idea is to inject them (although it may not matter a whole lot) - also when you evaporate your liquid you'll be left with the excess stuff as contaminant[/quote:45a911adb3] So is there no way to clean these contams out? Or are we still brainstorming?
 
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merely brainstorming (well i am at least) those contaminants i mention in the case of excess acetic acid would be pure acetic acid which is hygroscopic so you'd likely end up with a puddle with dmt crystals floating around as tartaric acid is a white powder in its pure form, i guess any excess tartaric acid would result in your amount of dmt tartrate + some tartaric acid. There may be some solvent which will dissolve one and not the other which you could use for separation. I bet there's probably other ways to separate too, but i'm not sure as water (distilled) is generally inert, it would be the solvent of choice to perform the reaction in. I *think* you can use the molecular masses to figure out how much of each to add in order to minimise excess of either: Molecular Mass of DMT: 188.269 g/mol Molecular Mass of Tartaric Acid: 150.087 g/mol So for 188.269 mg of DMT base you'd use 160.087 mg of Tartaric Acid put into a solution of about 10mL distilled water i think would be enough and stir. Evaporate under minimal heat and that should work Alternatively, perhaps a more volatile solvent (but still inert) could be used so you could just evaporate in air to leave the product.. Is IPA inert? (i'm pretty sure acetone is quite reactive)
 
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