clean unused xylene is precipitating when FASA added.

[sawman87]

hi all,

okay so my first question here which i cant find an answer for...

i have precipitation in clean unused xylene when adding FASA. hopefully someone can tel me why? or what it might be?

i have too much dmt fb on hand that i want to convert to fumarate. i prefer oral journeys.

i usualy use naphtha as my solvent but have read that fumaric acid precipitates out of it alone. and some other solvents cause this also. so i want to use xylene to disolve some of my freebase and add FASA to get dmt fumarate.

i decided to test the xlyene first by adding filtered FASA to unused xylene straight out of the unopened tin. i added FASA slowly and cloudiness appeared instantly. the next morning precipitates were on the bottom. is this normal? from what ive read on here so far i didnt think it should. i hope the precipitates are just fumaric acid and not something else out of the xylene. if so i think i will end up with a mix of dmt fumarate and fumaric acid.

thinking about it now, would it just be better to disolve freebase in acetone and then add FASA to that drop wise?

or i could go ahead and use xylene. if it is fumaric acid preciping out a acetone wash after would remove excess fumaric acid and leave the dmt fumarate.

okay i may have answered my own question. so i think what i need help with is... is there anything that could be in the xylene that is precipitating out? or do i forget it and do the acetone method?

any help would be very much appreciated.

 

[downwardsfromzero]

thinking about it now, would it just be better to disolve freebase in acetone and then add FASA to that drop wise?

For best results, it's important to ensure the acetone is completely dry. I could be guessing here, but damp FASA may be responsible for the precipitation in your xylene.

If you're not pulling from an aqueous phase, it's not strictly necessary to use xylene. Plus acetone smells rather better than xylene!

Adding dry acetone to limonene before adding FASA seems to help prevent precipitation of fumaric acid; the same might apply to xylene. But in that case you might as well just dissolve the freebase in acetone seeing as you're not doing an NP extraction here.

 

[sawman87]

hi, thanks for your reply.

my acetone bottle says its anhydrous 100% acetone. so there should not be any moisture in there.

i think il go the FASA into dmt acetone route then. thanks for the tip on adding a little acetone to limonene. i may need that one day.

in future i may continue to pull with naphtha and freeze precip. then disolve in acetone and add FASA.

Many thanks

 

[downwardsfromzero]

Once you've opened that bottle, it's had a chance to absorb moisture from the atmosphere, unless you opened it in a dry glovebox or something similar.

 

[1ce]

If you have acetone then why are you monkeying around with xylene?

 

[endlessness]

That's really weird!

It def shouldn't precipitate... It beats me why that would happen. I don't think a small amount of residual water would do that, but I could be wrong. At the moment I'm way too busy to run tests, but yeah if I were you I'd dissolve freebase in acetone and add FASA to that.

Good luck, and keep us updated!

 

[sawman87]

If you have acetone then why are you monkeying around with xylene?

good point. i guess i was just trying / thinking about all my options. see what works best for me.

i normaly use naphtha freeze precip then redisolve in xylene if i want freebase crystals as it evaps quicker and leaves no trace when i did an evap test. my source of naphtha is very very long to evap and also it left very slight residue when i evap tested. i know i could use xylene as the solvent to pull. but i understand this would also pull other actives present like n oxide. i prefer just dmt for vaped travels at the moment.

the freesbase i have at the moment i did patiently evap from naphtha but im sure its left traces. it doesnt taste right when vaped and has put me off vaping it. hence why im changing this lot to fumarate. i wanted to try the fumarate oral route anyway.

so could i use acetone as my solvent to pull dmt out of the bark mix? then filter the acetone and add FASA straight to it to get fumarate? although i understand this will give me other alkaloids also in fumarate salt form eg dmt-n-oxide fumarate and others. i use MHRB with Q21Q21'S vinegar lime a/b tek. normaly with naphtha.

 

[endlessness]

Nope that doesn't work well.. First of all you'd have to basify the bark before the acetone.. But even then, I tried it, nothing precipitates. I think the impurities prevent the fumarate precipitation. You could possibly instead evaporate the acetone off, then purify the resulting product in any number of ways (for example dissolve in small amounts of hot acidified water, filter thorouglhy with funnel and cotton plug, then evap/mix with sodium carb and let dry, then pull with acetone again) and then FASA it after the clean up.

As for dmt n-oxide, for the most part I think it will not be there, I hardly ever detected it in any of my tests, I think people used to say n-oxide a lot becuase they related goo to oxide but that is not necessarily true, even pure dmt (and/or nmt) can be a goo/oil. Either way whatever it is, as long as the chems you used are good and so is plant material, you will have some nice product

 

[1ce]

Nope that doesn't work well.. First of all you'd have to basify the bark before the acetone.. But even then, I tried it, nothing precipitates. I think the impurities prevent the fumarate precipitation. You could possibly instead evaporate the acetone off, then purify the resulting product in any number of ways (for example dissolve in small amounts of hot acidified water, filter thorouglhy with funnel and cotton plug, then evap/mix with sodium carb and let dry, then pull with acetone again) and then FASA it after the clean up.

As for dmt n-oxide, for the most part I think it will not be there, I hardly ever detected it in any of my tests, I think people used to say n-oxide a lot becuase they related goo to oxide but that is not necessarily true, even pure dmt (and/or nmt) can be a goo/oil. Either way whatever it is, as long as the chems you used are good and so is plant material, you will have some nice product

This is true. I've tried evaporating a light solvent over distilled water to see if xtals would fall through. Unfortunately my 'xtals' wound up as a goo stuck to the sides of everything.