Ahoy.

Hoping for some answers on this zinc reduction.

1) Started with approx 6 grams of gooey n-DMT-oxide*.

2) Added ~120 mL of water and enough phosphoric acid to reduce pH to 2.7. The oxide dissolved into an amber coloured solution.

3) Added 6g of zinc powder, shaken occasionally in warm water bath for 2 hrs. Solution went clear.

4) 24 hours later there are needle-like crystals forming. They don't easily go back into solution with some gentle heat.

Must be DMT-phosphate, yeah? They certainly aren't zinc phosphate. And how would one get them back into solution to separate from the zinc?



--
* How do I know its n-oxide?
Amber oily goo, will not dissolve in naptha. Formed during hot naptha pulls, and would present with n'n-DMT crystal during freeze precip. The precip would never properly crystallise (nelting crystals) due to presence of oxide, so would be re-dissolved in hot naptha, re-precipitated, and then even more n-oxide was present (fewer crystals). I believe the hot naptha was oxidising the DMT upon each successive dissolve-crystallisation. Psychoactive.

It is most likely zinc phosphate. DMT phosphate would readily dissolve in water.

What you describe, the melting crystals, oiling happens with pure DMT. No n-oxide present. You should of tried to xtalise it further instead of reducing. You should also use acetic acid not phosphoric for this. Zinc acetate will reduce. Zinc phosphate won't.

Thanks for the reply. If you are correct @famine, I guess one could simply decant, basify, and attempt to crystallise once again then.

Yes decant, basify and pull with organic solvent