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Interesting crystalization method

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Brennendes Wasser

Brennendes Wasser

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Senior member Chemical engineer
Somewhere I read about a crystalization method, that is super easy to conduct, but sounds quite effective.

It was called something like diffusion-based crystalization and thats how it works:

Get a big glass container and place a concentrated solution of your Compound X dissolved in Acetone (or any other medi-polar stuff) inside of this container.

Beneath you place any other unpolar, very low boiling solvent in an open container. You could use Diethyl ether or Pentane.

Now just close this completely and wait - the low boiling NPS will evaporate and of course also migrate over into your vial of desire. Then your Compound X may ultimately precipitate very gently.




So ... of course this will not work with DMT, as it is also solubly in Ether and the solubility in Pentane is also not completely 0. But I think this may work with more polar things, that are hard to crystalize, like 5-OH-DMT or 5-MeO-DMT. Then again Pentane instead of Ether should be used. But so far no idea if it would work even for them ... :?
 
That is a nice, simple technique. It would indeed be tricky to get it to work for plain DMT - addition of even a fairly small amount of acetone to naphtha completely prevents it from freeze precipitating, for example. Perhaps a reverse version could work - dissolve the DMT in the low-boiling solvent (pentane?), seal it in a container with a separate amount of high-boiling naphtha and the low-boiling stuff should diffuse into that. This reduces the amount of solvent that would get lost through a simple evaporative crystallization.

In a broadly similar manner though, I've considered using a diffusion method for precipitation of freebase harmalas from a solution of their salts. Instead of a low boiling polar solvent, one would use concentrated ammonia solution. The ammonia diffuses into the harmala salt solution and large needles should form quite slowly.
 
Found out by accident that 5-bromo-DMT freebase recrystallizes quite nicely in from methanol if you dissolve it in methanol and then let the methanol evaporate off at room temperature.
 
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