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freezing dry iso to precip fumarates

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mew

mew

huachumancer
given that my dmt fumarate was a chunk and not easily powderable i decided to use warm dry iso to dissolve it,
i put it in the freezer and 2 days later there is a cloud of white settled on the bottom

after careful decanting this amount will be evaporated to hopefully yield dmt fumarate without excess fumaric acid


this should work right?


additionally this dmt was extracted form aya that had been decanted for 6 months, just recently it had the harmalas precipitated before dlimo was used to pull the tryptamines. the brew was fully active however too much acetic acid was used and it sat neglected (decanting every so often) in my fridge. given i have an awesome brew of aya fresh i wanted to see if could use washing soda to successfully freebase dmt and see if i could precipitate contaminant free fumarates as i salted with fasw . the fasw was evaporated and turned into a chunk thats what was dissolved in warm iso


what i didnt see coming was that the precipitates from freezing at first were a cloud and would definitely escape anything but a micron sieve, which i dont have. so i let them sit another 2 days to hopefully grow and settle. which they did. still it seems that the yield is moderately insignificant
 
Maybe your iso wasn't very dry or you used too much. I'm not fresh on solubility of dmt fumarate in isopropyl alcohol though, or if what you have done is commonly done or not. One thing I would try before assuming all hope is lost is add some d-limo or similar solvent(toluene, xylene,etc) that will mix(miscible) with the IPA. Try adding a few drops and see if the solution becomes cloudy. Or add a few drops of the IPA with dmt fumarate to another solvent(small-scale) so you don't taint your stuff with d-limo for something that won't work(if it works it should get cloudy). Make sure the solvent you use will mix with IPA first though.

What this should do is lower the solubility of the dmt fumarate by making the solvent(IPA) more non-polar. I would suggest letting it evaporate some but it likely will become wet by doing this(pulling moisture from surrounding air).

Not 100% on if this will work but I think it is a good thing to test, before assuming all hope is lost and having to evaporate the whole thing and starting over.

Thanks for experimenting.
 
Yes, fumarates are soluble in hot isopropanol, so you will need to use only the absolute minimum amount of boiling solvent needed to fully dissolve your salt. Its very easy to add too much.

Crashing out your fumarates out with another non-polar solvent is a sound strategy, but do it very slowly, dropwise with ice cold solvent. Also your non-polar solvent should not be extremely non-polar (ie naptha or hexane) or you will end up with two layers. NP on top with salt saturated alcohol on bottom.

Ether would be sisters choice of NP if you have access to it. It can be purchased OTC as cold starting fluid from an auto supply.
 
Dr sister are you positive on fumarates being very soluble in IPA? I really dont think so, Ive used cold/room temp IPA to wash fumarates and they dont dissolve in it, or just barely if so.

Personally the IPA re-x and acetone re-x never really worked well for me, either they didnt dissolve or once they did they never seemed to crash out, only being a fine cloud that didnt get filtered. What I do to clean up fumarates is explained in the sticky in the fumaric acid subforum, its basically freebasing it by mixing with sodium carb and bit of water, drying, and pulling with acetone and doing FASA on it. That way it crystallizes again very clean.

And mew, I would think that the stuff you decanted away from your IPA would also have dmt fumarate.
 
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