FASA -> toluene produced milk and yellow liquid, what do i do next?

[drpotato]

I added FASA made from mg sulfate dessicated acetone that had then been distilled (after decanting, not distilled with mg still in there), added fumaric acid and made a solution with lots of acid still settled in there to ensure it was truly satured, let that sit with mag stirring in a GL45 for a few days.

my toluene extract of 100g acuminata had been distilled down from about 150ml to 60ml, to make it nice and conc but also azeotropically remove any water.

I added the FASA to the toluene which i also spiked first with a little dry acetone as i heard that helps. at first not much happened, then additions of FASA produced dense clouding, was very happy seeing this. i ended up adding 40ml, this is much more though than the expected yield. I have been waiting for several hours and the solution remains cloudy with nothing settling out, until i noticed the formation of a yellow liquid.
Also ill note that until i transfered the beaker to a dessication chamber it has been under cling wrap and hasnt spent more than a few minutes exposed to the atmosphere, its quite humid here.

yellow liquid continues to form.


Additionally, when concentrating the freebase pull at first i ran it a little too hard and the solvent was distilling a bit of smoke, not much though, and not for more than a few minutes either, but the recovered toluene, about 200ml does seem to smell amine-y when dried so i decided to add fasa to that as well. i added a bit of dry acetone at first since it also contained droplets of water, due to azeotropic distillation and all. same effect, only very big fluffy crystals formed, for maybe 5ml of FASA, and after that no more. whats odd though is, this was very wet toluene. just to confirm fasa doesnt just crash out or something i added some to some unused toluene and while it went a little milky, no crystals formed.


So, can someone explain what happened?

theres a dozen ways acetone can spontaneously wet itself, is the non-settling milk a dispersion of liquid DMT fumerate? or did an aldol condensation occured and this is some phenomena due to diacetone or other condensation products?

what should i do next, what is the timeline here? somehow the wet toluene also produced a pretty instantaneous precipitate, but it seems more like what one should expect, but in the main beaker, i just have a yellow milk with goo coating the glass all over. would stirring help? heating? cooling? or just waiting?

 

[drpotato]

update - the solution has gone clear now, im not sure if stirring helped or not. the DMT fumerate has formed a solid, its like hard-candy or that snappy kind of taffy that bends like tar real slow and snaps and crushes like glassy traditional hard candy would.

but also, the FASA+pure toluene has also yielded precipitate, so now im not sure how to enterpret this. its small grains like fine sand, wheras the precipitate in the flask with the DMT fumes, were light and fluffy.

After doing more reading i have discovered that IPA can dissolve DMT fumerate, and i can use it to do a recrystalization in a similar kind of manner to hexane. boiling off the residual toluene will also pull all the water out too, as IPA, water and toluene torm a ternary azeotrope that is 13% water, so provided i can dissolve it all, the water should be driven off and ill have nice anhydrous solvent.
going forward i think i might just use toluene+IPA from now on, and do FASI, for water to be in my acetone means the acetone underwent aldol condensation, to form water, because it got dried too hard that it self-wet smh

 

[drpotato]

could someone delete this? ill rewrite this experience as a new post, along with my results since the DMT has now been cleaned and freebased