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Precipitation of DMT out of chloroform Options
 
Dozuki
#21 Posted : 1/8/2012 11:48:01 PM

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Thanks for that, I'm not sure that there should be a link directly to the DEA on the board however. The title of the paper should suffice Pleased

After reading the paper, I am very dubious of their claim that the AcOH procedure produced a "crystalline product". They may be intentionally leaving parts of the process out. Also, the use of CH2Cl2 and MeOH is not very specific for DMT. AcOH, especially at 3% is also not a very specific solvent as the H2O will drag the polar components out.

 

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Madcap
#22 Posted : 1/9/2012 12:56:33 AM

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benzyme
#23 Posted : 1/9/2012 1:12:29 AM

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Adivino wrote:
the precipitate is a brown oil


did you dry your solvent over a sulfate salt?
it may be a supersaturated solution of hydrophilic compounds
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Adivino
#24 Posted : 1/9/2012 2:13:32 AM

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Yes, I dried the chloroform with MgSO4, which already resulted in an oily substance when evaporated. The recrystallization from pet ether (which was not dried) gave the same thing.
I will abandon this extraction, since it's a very small amount anyway.

I'm going to try again using a more specific procedure:
Reflux for 30min finely powdered mimosa in 3x 96% ethanol with frequent hand agitation, combine and evaporate. Redissolve in water, basify with NaOH to pH 12-13 and extract with chloroform once or twice.

Now the part which I'm not sure: I was thinking of adding a saturated solution of salicylic acid in chloroform to precipitate DMT salicylate. Has this been tested? Salicylic acid is somewhat soluble in chloroform. I'm having a hard time getting fumaric acid. I don't want to evaporate the chloroform and risk obtaining some probable N-oxide again.

benzyme, you say that you evaporate the chloroform and recrystallize from pet ether, but how exactly do you do this?
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benzyme
#25 Posted : 1/9/2012 2:19:11 AM

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after you evaporate the chloroform, you should have a reddish/salmon colored resinous product.
heat up some pet ether in a hot water bath, then dissolve the product with it. transfer that to the freezer. after a few hours, the product should crash out.
when you decant off the pet ether, you'll be left with light-salmon colored crystals.
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Shaolin
#26 Posted : 1/9/2012 9:09:57 AM

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Internal link for the DEA paper.

Adivino, I'm a little confused why would you combined the methanol and acetic extractions ? Potential yield increase ? Or a you hunting for some specific compound ?
Got GVG ? Mhm. Got DMT ?

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Adivino
#27 Posted : 1/9/2012 5:44:18 PM

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Shaolin, yes, as I understand it, acid ethanol disrupts plant cells more easily. This may not be necessary with mimosa, though, and I'm only desiring to extract DMT. It's just experimentation.
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