I'm prepping a compound from literature, and the ref. calls for purification on silica using DCM/MeOH/AcOH as mobile phase. The compound looks OK but there is tons of AcOH and MeOH still present by NMR, even after 3 days on high vac. Is there a trick for removal of AcOH similar to azeotroping water away with toluene? Extraction is not an option as the desired product is also a carboxylate. Moreover, the next step is to amidate the carboxy group, so I think I need to remove the acetic acid.
Any advice appreciated!