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purifying by pulling it back into acid

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T

tryptographer

tryptamine photographer
Has anybody tried this yet:

- basify the MHBR powder and extract with the naphta like in standard STB
- then, instead of freeze-precipitating it directly (and/or evaporating): add vinegar or dilute HCl to pull the alkaloids into the polar layer. Some fatty contaminations should be left behind in the naphta.
- basify the acid solution with sodium carbonate and extract again, with clean naphta
- freeze-precipitate this
I'm going to try it with a small batch, say 50 grams and will report back how it went and take some pictures. It's just a small extra step and I suspect it's a good cleanup.

I did some purifications of dirty brown spice before by re-dissolving in acid, defat first with toluene and then naphta, basify and finally pull back with naphta. It's fun to watch the milky-whitish DMT fall out of solution, in the black sludge you see nothing like that!
 
OK, a quick status report...

Took 25 g of root bark, added this to a flatbottom flask with 250 ml of water; added 30 g of slaked lime - a paste of moist Ca(OH)2. Put this flask in a hot water bath and let it simmer for two hours. (1st pic)
Still hot, I added the naphta, swirled well for a few minutes and sucked it off. To check if there was something in it, I took maybe 10 ml of this and put it into the freezer. It started to get turbid quickly, a good sign... next day some shiny snowwhite crystals (3rd pic).
OK, there is something in there, the lime tek works! And it produces pure white crystals, not a hint of yellow, a stark contrast with the lye tek. Snow-white glass shards in just one step!

Just to test the initial idea, I added 4% HCl to the naphta to get the DMT back into the polar phase. Not really necessary but I want to see if the idea is valid...
After separation, the acid was basified with sodium carbonate. A lot of bubbling from CO2 escaping, then then whitish stuff precipitates. Good! (2nd pic)
Added some clean naphta to extract back into non-polar and this is now in the freezer, slowly getting turbid. I also took a bit of the hopefully exhausted naphta to compare, it should have hardly any dmt left. So far so good, it's still clear after a few hours in the freezer.

The only dubious thing so far is that there still is precipitate in the acid after the naphta extraction. I wonder what it is, did the naphta and the HCl pick up some calcium??
 

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My friend tells me he tried this using mimosa, lye, water, and muriatic acid.
He says it worked as he hoped. Both times he's tried..

As for the left over precipitates, he doesn't know.
He uses only lye as a base.
 
Hm, this turned more into a lime vs lye experiment than the subject suggests...
Anyway, this pulling into acid seems to work well, vinegar instead of muriatic should be ok too.

I found out that this precipitate is a contamination in the cleaning soda that's sold in the nearest super market. It doesn't even make a clear solution in distilled water. Next time I'll basify the acid with ammonia or lime and see what happens.

Meanwhile, I tried to extract from a dried lime/mimosa powder paste with warm naphta... no success!?? I'll also check with acetone. Should have defatted the powder first.
 
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