First of all,
in situ MeAm gas generation is normally accomplished with a solvent
not miscible with saturated aequous salt solutions. MeOH is miscible with NaCl/H2O, so I would advise you to use EtOH, iPrOH or even better a nonpolar like hexane or toluene here. See Barium's "wet method" for details...
Next thing is that the MeAm solution mustn't become hotter than 15-30°C, or else the gas will escape and you'll be left with a maybe 5% solution instead of 10%...
Also, I would rather add the ketone before basifying the methylamine.HCl - the 30 minutes before NaBH4 addition are not enough time for the imine to form. And the imine formation occurs preferably when the formed water is removed - this is accomplished
in situ by the generated NaCl; it dissolves in the water from imine formation, forms a very polar solution, and the amine/imine/ketone containing solvent becomes immiscible with this polar NaCL soln. Therefore my advice of using a np solvent...
And I really wonder about your crystallization: WHERE THE HELL did you get 50% HCl?
![Smiley :)](https://thevespiary.org/talk/Smileys/default/smiley.gif)
AFAIK 37% is the highest concentration possible! Or did you mean a pregassed 50% alcoholic HCl solution?
indole_amine