yes it should have been followed to the "T", but I was thinking along the lines of "No big deal if I get a lower yield of lower purity" what I didn't realize was how incredibly those purification steps are. The acid/base extractions I thought would have given pure enough product with some yield, but, for whatever reason, skipping them
left me with nothing. A few points that are a bit vague in the paper 1) Under the experimetal section for ::: rac-Methyl 4-(4-Chlorophenyl)-1-methylpiperidine-3-
carboxylate (1, 2).The crude mixture was crystallized from EtOAc/hexane ::: So I assume it is dissolved in a min amount of EtOAc, heated, then hexane is added until the solution just turns cloudy, a drop more EtOAc is added to make the solution clear and it is cooled down slowly with stirring then put into an ice bath to recrystalized. Comments?
Under the same section
2):::::
The hydrochloride salts of these compounds were
prepared by dissolution of the free bases in a methanolic
solution of HCl(g), concentration, and final trituration of the crude salts with ether::::. So it seems that one pre-gasses the methanol, then disolving the freebase in this methanol. But what of the concentrating and "final trituration" with ether? Is this a fancy way to say wash the resulting hydrochloride crystals with ether (I assume they fall out of solution when the pre-gasses methanol hits the free-base)?
Anyways my project was a failure, hope someone else tries!