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!
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!