Sciencemadness Discussion Board

crytallization problems

chemrox - 25-8-2010 at 22:00

I've made a heterocyclic amide ester, mw ~ 510. I isolated and collected the base. It was a gummy pale orange solid. Color due to impurities. Without purification I weighed it and dissolved it in THF/MeOH. I made the citrate but after a dozen or so solvent combinations was unable to ppt the citrate. I then recaptured the base and tried to make the HCl as follows- I dissolved the base in ether and then added con HCl in ether. Beautiful white crystals formed but my vacuum filtration wasn't quite ready and all the crx disappeared in the refrigerator forming two layers of liquid.