Thanks for your info, Barium. Just read that dithionite reduction gave you ~1% P2P contamination, compared to ~20% P2P resulting from hypophosphite-Pd/C rxn... Dithionite seems to work somewhat cleaner. Hm. Using acetone to affect complete hydrolysis sounds good, but I thought the purpose behind ketone formation was to bee able to separate via steam distillation and to avoid having to solvent xtract (unless the reason is that you NEED ketone, not oxime)? Wouldn't acetone interfer with this?
Oh, and about basifying tin with ammonia: I think tin will normally give a mess upon basification, too (read somewhere that workup of Na
2SnO
2 reductions to oximes is very hard, and I thought that was the reason why aurelius suggests hydrolyzing w/HCl - to simplify workup?) so I thought Rhodiums idea would perhaps solve the tin problem, too...
Does tin form complex salts with ammonia? Are they less soluble than hydroxides in nonpolars?
Nicodem:
THX
seems as this method isn't very popular at the hive, I really don't know why!?
And do you have any references for your idea of an anhydrous Zn/HCl reduction? I'm asking because I perhaps may have use for this doublbond-halogenation for some other, eeasy procedure if this really works...(secret)
A