chemrox - 1-2-2007 at 23:20
I followed a procedure for obtaining an HCl salt by azeotropic distillation. The solvent was water in xylene. The xylene amount was supposed to be
10:1. I cut this to 4:1 based on a previous distillation of the two components. Big mistake. At close to the end the free base started getting
fried and coming over. What a mess. I may be able to salvage some of the product with norite and a/b extraction. The thing that bothers me is why
would the HCl separate and release the base? The aqueous solution was strongly acidic prior to the distillation. Please be kind, this hurts.
Maya - 2-2-2007 at 05:07
it doesn't , salts don't distill ( unless it is an ammonia salt or a methlyamine salt ) you fried your compound. now its obviously something else.
try using a lower temperature or something other than xylene 
[Edited on 2-2-2007 by Maya]