sup everybody. guess im still stuck as new member so im gonna shoot my shot right here hope y'all dont mind

basically a buddy of mine is doing this tek right here to turn his fumarate into freebase:

https://wiki.dmt-nexus.m...p_6-Fumarates_conversion

he had it sitting in a buddies fridge. was supposed to pick it up but buddy got the text late and long story short left that shit got out overnight. all the formed sediment went away - sad face... apparently even after several hours sitting in the fridge, still no where near the amount that was there originally - even sadder face...

so he just wants understand what happened out of pure curiousity. it would seem that the warm conditions led to a shift in equilibrium which completely reversed the reaction... but in order to confirm this it would be required to first confirm the reaction which occured, as well as, the bond disassociation energies

including a photo of the reaction proposed by my buddy. any info y'all can offer would be very helpful to him - happy face

Proposed Rxn

If you could nonetheless write out exactly what was done it would be easier to comment.

The reaction itself is nothing special, just removal of a proton from the amine nitrogen of the DMT. There's no need to be thinking about the bond dissociation energies on any kind of a practical level. The main thing to note is that the carbonate anion acts as a base w.r.t. water, forming bicarbonate and hydroxide. The hydroxide removes the proton from the amine, more or less. Given the addition of sufficient base, the reaction will run to practical completion. Because bicarbonate is only a weak base, two equivalents of carbonate are required to react fully with a given amount of fumarate - slightly more than two, in fact, due to the absorption of carbon dioxide that occurs.

Thus, one possibility is that the basic solution has absorbed carbon dioxide, causing the freebase to redissolve. You could always try adding a bit more base, putting it back in the fridge and seeing what happens. It also could be that the crystals are fewer in number but larger in size. That might make it look like you have less yield.

A definitive way of retrieving the freebase from the solution would involve using a suitable solvent at a suitable temperature. Whichever way you proceed there will be some losses.

I just took a look at the fumarates to freebase conversion tek you linked and was shocked at how different that sequence of images looks to my experience doing the same thing. Its especially surprising because it that exact tek that i first used years ago, but then did my own developments to refine it since.

So i will share my interpretation of how to do this conversion.

First you need a lot of saturated sodium carb solution. About 1:1 with your fumarates solution. Second no fridge necessary. I never use mine and i get 100% conversion yield every time. What will happen is a caramel oil will start to form and try to float to the top. If you get a ring of caramel lower than the top, then put more base in. I find that after putting 1:1 sodium carb in adding a small amount of NaOH to push the pH a bit higher speeds up your result.

There's two approaches from here. Wait a few days for the oil to harden, which takes less time if you added that bit of NaOH. Or, perhaps preferably, lift the caramel floating goo out of the water and onto a glass evaporating dish. It will dry surprisingly quickly. The act of taking some goo out, will encourage the remaining goo to harden quickly on the water too. So its win, win for time.

Now, in either case, the resulting freebase will be about 10% sodium carb contaminated. So you must re-x. Simply get some dry acetone, dissolve your freebase into it, and the sodium carb will drop out. Pipette the acetone away from the sediment for incredibly pure freebase.

Enjoy


PS Thanks DFZ for that explanation of how sodium carb bases, I had no idea. Always good to know whats happening behind the curtain!

1:1 mol ratio?

what is a "little bit" of NaOH?

oh no doubt that sounds easy as hell. is it still gooey after re-x?

ok i told him this and he said he added 140ml warm distilled water with ~17g sodium carbonate

unfortunately no bubbles seemed to appear like last time, presumably because of the lower concentration. hope some good comes of it, hes trying so hard

1g fumarate -> 40 ml distilled water (followed by decanting)
~7g sodium carbonate -> 100 ml distilled water (warm)

sodium carbonate solution added dropwise over the course of four hours. left in fridge for 6 days or so then left outside in 78 degree F weather. solid disappeared.

followed up with steps in previous comment

So looks like this is all he got from that last attempt that seemed to reverse after warming outside overnight.

Should they also do the acetone re-x on this? Looks like there's not much of anything there. Also its on a shitty coffee filter and it looks like it'd be difficult to properly separate without dissolveing. Might also be best to wait and see what is produced by the most recent addition of more base does.

To be clear, what you see is what they filtered out before the addition of more base.

Is this a suitable source of NaOH? One bead = a small amount?

bump