Troubles converting fumarate to freebase

[thedivinesolvent]

I followed q21q21's tek and extracted using xylene and salted out using FASA. I let it sit overnight and scraped out the crystals on the bottom. Total yield was around .5g fumarate.

To freebase, I dissolved the fumarate into water in a shotglass, which gave a clear yellowish solution. Upon adding sodium carbonate, some bubbling occured, but nothing else. 15 minutes later, still yellow and very clear. Maybe it wasn't a strong enough base so I added some calcium hydroxide. This caused white powder to settle to the bottom, which could be excess CaOH. Evaporated and dissolved as much of the white/tan powder into acetone, and evaporated that. Got a very small amount of red goo. I'm not sure what to do with this.

In a later pull, dmt fumarate was obtained again. Dissolved into water and got a yellow solution that was cloudy. Nothing settled to the bottom however. Added sodium hydroxide since calcium hydroxide has poor water solubility. Again nothing happened. If anything, the solution became clearer when I added the base in.

Am I doing something wrong in my attempts to convert DMT fumarate into freebase? I feel almost as if the crystals I collected are just fumaric acid and there is no DMT present?

 

[JilPil]

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[thedivinesolvent]

Did you use fumaric acid to precipitate out the DMT from the solvent? If you did that you should have DMT fumarate crystals that settle to the bottom, not any goo. If you used vinegar to salt it out, then you will have DMT acetate which will need to be heated with a spoon to freebase. To freebase DMT fumarate, the general consensus seems to be to dissolve into water and add a base like sodium carbonate which will cause freebase to precipitate out. For some reason I have gotten the DMT fumarate to precipitate out of solution easily, but I haven't been able to turn it into freebase.

 

[Plainoldsteve]

Steves friend is having same issue with the sodium carbonate saturated solution, anyone know what's up?

 

[endlessness]

Cryatallization can potentially be affected by different factors.

First thing to do is not to start improvising. Calcium hydroxide is not a good base to add in this case because it is poorly water soluble so even if your freebase dmt crystallized it would be mixed with the indissolved calcium hydroxide.

Also, you didnt describe how you added the sodium carbonate. Straight to the solution? Predissolved in a saturated solution which was later added to your dissolved dmt fumarate?

Always make a sodium carb solution before, and add the solution very slowly, dropwise, to encourage slow crystallization which will mean nicer crystals.. adding it too fast may mean very tiny crystals or none at all (i think some impurities may interfere with crystallization)

To recover from mistakes, you can pull everything again with xylene or similar non polar and salt out again and repeat the process correctly, or you can instead do a paste with your fumarates and some sodium carb, pull with acetone or IPA and evap that.. im pretty sure these different conversion methods are well described in the BLAB tek in the wiki.

Good luck!