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Psilocin freebase to fumarate - what did I do wrong?

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Is it possible that psilocin fumarate is too soluble in etoh, especially with that 4% water? In terms of polarity, its water first, methanol, ethanol, iso, and lastly acetone. That's why tone works best for doing this. Even if you had dry etoh, perhaps it still would not crystallize since etoh is a fairly polar solvent to precipitate crystals out of.

Then when it evaps, maybe the fumarate is hydroscobic to a degree, and it prevents crystallization just like with dmt fumarate and water, it evaps to a goo before crystallizing. Or you have to wait a day or two for it to crystallize.

If you can't get dry acetone, perhaps if you can get 99+% iso it would work.

I bet its the water, and the higher polarity of etoh causing crystallization to be delayed, or prevented from occurring at all (if the fumarate is at all hydroscobic).

But thats just speculation, i do know that fasa with 4-aco/ho in dry acetone works very well. And i was able to base it with lime, which tops out around ph 12.4, seems like the magic spot according to that chart. I noticed little degradation converting gooey brown 4-aco hcl into mixed psilocin/4-aco fumarate salts. Psilocin because i think a good portion degraded into it as it turned into a goo and in the base hydrolysis when i based it with lime paste. It was just as active (qualitatively different though) per mg as white 4-aco fumarate that had not degraded. If you work fast perhaps it prevents the "amine side chain likes to bite back and hydrogen bond with the 4' phenol", that was mentioned by joe dirt.

All speculation though. :? :lol:
 
Thanks for the suggestion. Trying it with isopropanol was indeed the next and last thing I was planning to do.

So, you're saying I should evaporate, or crystallize in the freezer?
 
Important question: does it really work using a 1:2 molar ratio? Someone suggested it might not be so. Is it really established that the other 4-substituted tryptamine fumarates (4-AcO-DMT, 4-HO-MiPT, etc.) have two molecules per molecule of fumaric acid?


Here are some links I've found that seem to be relevant for this, but I don't know enough chemistry to really decipher them:

"As a potential replacement for (1), 4-Acetoxy-N,N-dimethyltryptamine fumarate (2) was conveniently prepared by shaking under hydrogen a mixture of 4, acetic anhydride, and sodium acetate in benzene with Pd/C in a Parr low pressure hydrogenation apparatus. Following uptake of the required amount of hydrogen corresponding to O-debenzylation, the catalyst and insoluble salts were removed by filtration. One molar equivalent of fumaric acid was added to the filtrate"

^ Check out the molecular diagram - it shows only one psilocin molecule to a fumaric acid molecule.
 
I've always heard that tryptamines form difumarates w/ fumaric acid. 4-ho met, 4-aco-dmt, 4-ho-dmt, etc. One fumaric acid molecule to 2 tryptamine molecules. With dmt it works out to 22-25% b/weight.

I've also heard that mono-fumarates can form, but i'm not sure how that would work, or if it only happens in certain solvents when its precipitated a certain way. Using %30 by weight of the freebase using fasa/fasi should work out pretty well. No excess FA will be present assuming you do fasx, but evaporating the solvent could leave residual fumaric acid if you used a little extra than what was needed.

Found this on drugsforum-


2) Fumaric salt:

The formula
2 X (4AcODMT) + 1 X (Fumaric acid) = Fumarate salt

The masses
492 + 116 = 608

The percentages
80.9% + 19.1% = 100%

Whereas the hydrochloric salt consists of equal parts 4-AcODMT and hydrochloric, the fumarate salt instead consists of 2 4-AcODMTs for every 1 fumarate. This is because fumarate is a divalent anion and carries two negative charges. Thus one fumarate can neutralize two 4-AcODMTs each carrying one positive charge.

Read more: http://www.drugs-forum.com/forum/showthread.php?t=149679#ixzz21pWnNKNs
 
Thank you, but I had been receiving contradictory advice on this, so in the end I figured it was better to risk having some excess fumaric acid than some unreacted psilocin that would degrade. Fumaric acid is harmless AFAIK, but psilocin is a rare and valuable substance. So, I added more fumaric acid to a 1:1 molar ratio.

I mixed them in isopropanol then evaporated. I obtained some DMT-like crystals that looked like bundles of needles plus a solid layer that could be scraped into a light grey powder.

The only problem I can think of is that if there is unreacted fumaric acid left, it is concentrated in either the crystals or the solid layer, and thus it means that the resulting powder has uneven potency and the dosing will be messed up.

Now, what remains to be seen is how stable the resulting substance is. All the other tryptamine fumarates are pretty stable. Is it possible that the reaction was somehow incomplete or unsuccessful and I still have some psilocin base?
 
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