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#1 Posted : 2/1/2014 1:02:58 PM
So I was preparing a FASA, 1g DMT freebase dissolved in 50ml acetone, 390mg fumaric acid dissolved in 50ml acetone. I poured the dmt solution into my precipitation glass, then realized it would be too small to hold the fumaric solution.

In my haste, I decided to just reweigh another 390mg fumaric acid and added it directly into the dmt solution with an additional ~20ml acetone.

I've done this before and didn't think it would make much of a difference skipping the step of pre-saturating a fumaric solution. But the precipitation was a lot faster than normal, almost instantaneous snow-like crystals (compared to the traditional, several-hour long precipitation of needle-like crystals) so I'm wondering whether the fumaric has properly dissolved and rebound with the DMT or not.

I stirred it while mixing and when it settles it looks like a nice pile of dmt fumarate on the bottom, but it was such an instantaneous reaction as I was adding the fumaric acid, so it's hard to say whether it's all dmt fumarate or could it instead somehow be oversaturated / undissolved fumaric acid?

If it's decided that there is undissolved fumaric acid contaminating the precipitate, how should I go about recrystallizing?

Thank you!
 
wearepeople
Senior Member
#2 Posted : 2/1/2014 3:57:55 PM
In light of the Gates of Registration being closed, I will give you a hint instead of the answer.

So what is the problem?
Fumaric acid contamination in your DMT fumurate

How would the problem be fixed?
Finding something that DMT fumurates are insoluble in but fumaric acid is soluble in.

How does FASA work?

Where would be a good place to read about this?
The FASA/FASI/FASW sub-forum

And what's the big hint?
I know you already have the solvent on hand, just make sure its cold & anhydrous when you use it.

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