100 grams of 5-MeO-tryptamine freebase is dissolved in MeOH with vigorous magnetic stirring. A thermometer probe is inserted into the methanolic 5-MeO-tryptamine, and the solution is cooled until it nears 0 °C. Aq. KOH is used to dissolve and stabilize 100 grams of NaBH4, and the solution is transferred into an addition funnel. A second addition funnel is charged with a MeOH-stabilized aq. 37% formaldehyde solution, and the drop-wise addition begins. "And now I start adding the borohydride." [...] Borate salts gradually precipitate, and the salt volume is reduced by overnight heating. As the methanol evaporates, 5-MeO-DMT precipitates as a brown oil and coalesces on the surface. "Pretty beautiful." Simple distillation is used to strip the remaining water, followed by purification of the crude freebase via short path vacuum distillation, "We did it. Yes.", and recrystallization. [...] After TLC had shown total transformation of the starting material, LC-MS confirmed the product was 5-MeO-DMT.
There sadly is some stuff missing in that synthesis, first of all if he uses Acetone/dry ice as his bath, then the reaction most likely will run below 0°C. Doesn't mention reaction time or amount of HCHO. Simple distillation may or may not carry along freebase 5-MeO-DMT. Also a bit puzzled how he can reduce salt volume by heating, probably meant to say solvent volume.
Not the most efficient or clever workup, but if it works, it's not stupid, right? ![Wink ;)](https://thevespiary.org/talk/Smileys/default/wink.gif)
watch it again.
he is adding dry ice cubes one or two at a time.
just because your using dry ice does not mean your reaction temp is below 0C
it all depends on volume of solvent reaction exotherm and how much dry ice to acetone there is.
he is probably just being lazy as it is easier to use a couple of dry ice cubes in acetone than an ice bath to keep an exothermic reaction
around 0 too 5C.
it also allows you to increase your addition speed.
tryptamine does not azeotrope with methanol.
methanol does not azeotrope with water and as you remove the methanol the salts will dissolve.
and finally the synth he is doing is well known so really he doesn't have to put everything down for a chemist to do it.
after all its just entertainment rather than a journal paper.
please don't pick on noobs its not becoming of you.