5-MeO-DMT crystallization (n-Hexane)

[Bubbles667]

Freebase was first pulled with DCM, after evaporating the solvent oily residue dissolved in boiling n-Hexane, when solvent cooled down a bit, seed crystals were used and precipitation occurred at room temp yielding beautiful, white shards of 5-MeO.

 

[Bubbles667]

Final yield: 1.89g from 5g of starting material

 

[Prima Materia]

Is the yellowish crystal a different polymorph as it is sometimes called?

 

[Bubbles667]

I think that’s exactly what it is, as there is no change in potency despite the color.

There is a difference in susceptibility to oxidation (losing electrons) between polymorphic structures, these yellow chunks are actually from later hexane pulls (which still gave white crystals, just in lesser amount), this caused one of the variants to oxides slightly, whereas the more stable one remained unchanged.

 

[Ruffles]

What was the starting material or source?

 

[Bubbles667]

5-Methoxytryptamine

 

[modern]

Is 5-meo dmt ph sensitive to high ph levels? would using lye be an issue even if ph is not extreme? like 11 range is enough. Asking here since not much info I can find elsewhere

 

[Bubbles667]

Is 5-meo dmt ph sensitive to high ph levels? would using lye be an issue even if ph is not extreme? like 11 range is enough. Asking here since not much info I can find elsewhere

It’s not a problem here, strong base like NaOH or KOH should be used and ph during acid/base extraction set above 11.

 

[neurobloom]

I remember this very synthesis from your reddit Post. Really awesome work! Crystalizing from boiling hexane usually leads to one oily phase at the bottom with a crystalline phase on top. The crystals can be harvested from the top and the rest of the oil can be recrystallized again. After a few crystalization cycles like this all the freebase can be turned into clean shards of glass.

But I'd say the best most straight forward way to get pretty white crystals is vaccume distillation..the distilled freebase oil spontaneously crystalizes as it cools down without need for solvent.

 

[Bubbles667]

Thank you !

Vaccum distillation is the best way to go about it ofc, although method described on reddit was deliberately simplified, so even someone without a decent pump (myself included) would be able to pull it off.