in a leuckart wallach reaction can formamide be used alone or do you still need formic acid as well.
if you can obtain pure formamide, you can use it just like it is. i use formic acid together with ammonium hydroxide to MAKE formamide. therefore you have to add ammoniumhydroxide to formic acid, until it is neutralized. then you have to heat it, to get formamide. use TFSE for further info on this topic, you should find a lot of posts.
im just a little confused as people seem to be using formamide alone but i dont see how this can be used as a hydrogen doner for reduction.
make some ammonium formate by heating the neutralized formic acid in a standard distillation setup and discard everything up to about 160 C. you should be left with a mix of ammonium formate and formamide, which i used with good results in leuckart reactions to make some mda. again use TFSE.
Added 46g MDP2P to 130g formamide (homemade) and placed in a flask sitting in an oil bath with glassware setup for normal distillation. Heated to around 170 DegC for 5 hours with stirring. After 5 hours, added 200ml water let cool and extracted into DCM. Separated DCM layer from aqueous layer and removed most of the DCM by gentle heating.
Added residue (with some left over DCM) to a mixture of 16ml methanol and 150ml 15% HCL heated to 60DegC. Evaporated residual DCM, then fitted reflux condenser and heated at around 80DegC for 2 hours with stirring. After 2 hours, let cool and washed with DCM. DCM wash discarded. Basified with 10% NaOH and 28ml raw MDA base fell out of solution to the bottom of the separating funnel. Extracted raw base with DCM, distilled the freebase and gased in xylene, yield 25g.
DF
