Excess Methylamine in gassing solvent

[chinacat]

Hi there,
could excess methylamine in gassing solvent interrupt the gassing?

 

[Marvin "Popcorn" Sutton]

It is best to get rid of the excess methylamine before acidification your base. The base usually has a strong smell of methylamine when it is present in great excess. To get rid of it, you can heat the base a little and stir it well, or rinse several times with warm ~40ºC water until the methylamine smell disappears. And then acidification with HCl.

 

[chinacat]

Do you think excess methylamine is the problem? could that be my issue? solved the syrup with dry acetone and xylene but defintely would prefer to go the dry gas route. Maybe that hydroxide wash may help or the solvent was just wet...which is possibe.. maybe will try letting it dry overnight next time.

 

[Marvin "Popcorn" Sutton]

I wrote a solution to the problem of excess methylamine. If the problem is precipitation when using aqueous hydrochloric acid solution, then you are right, you need to bind the water molecules with dry acetone or use dry HCl.
What are you synthesizing?

 

[chinacat]

MDxx compound,

So I vac distilled the freebase, added to IPA and managed to gas out magic crystals, I don't know what helped...but it helped. Happy happy.