methylamine syn needed

IndoleAmine · Dreamreader Deluxe

Cublium: the only difference between using hexamine and formalin/amm.chloride lies in the order of adding the reactands. If you add HCl to hexamine, it is hydrolyzed to formaldehyde and ammonium chloride instantly with heat evolution (so you should cool both HCl and aequ. hexamine solution before mixing them), you just have to add a bit more NH4Cl to compensate for the nonideal ratio of HCHO:NH4Cl of 3:4, and you also can add a bit of EtOH to create exactly the same conditions like you would have with MeOH stabilized formalin soln. ...

nubee: Tin(0) takes quite long to dissolve in HCl unless large amnt. of excess acid is used, since the concentration otherwise drops too fast to allow for continuous quick dissolution. You can add H2O2 to speed up the Sn(0)->Sn(2) oxidation, but IMO its a hassle to make (you also have to evap mucho excess HCl..). HINT: you can use a mixture of SnCl2/Sn/HCl for most reductions (nitromethane->methylamine!!), the generated Sn(4) together with Sn(0) dissociates into two Sn(2)... and it safes alot of work compared to converting all Sn to the chloride.... similar to Fe/HCl with catalytic FeCl3...

i_a

blackone · Fri Apr 29, 2005 3:08 am

Also an excess of NH4Cl would lower the percentage of dimethylamine created.

IndoleAmine · Dreamreader Deluxe

Exactly. Thats why one should preferably use some NH4Cl along with hexamine - to create an overall excess of amm.chloride (after the hex. has been hydrolyzed by adding HCl)....

If dimethylamine is desired, it is other way round of course - you'd have to add more HCHO.

Cub, did you already try using additional EtOH and distilling off the formed ethylformate at 52-54°C? It makes less side prudcts, really..

nubee · Master Archiver