反应详情

To the solution of venlafaxine base in isopropyl acetate from example 1 (66 ml, 10 mmol) 5 ml of 2 M aqueous HCl were added. The mixture was heated and water was removed by azeotropic distillation using a Dean-Starck trap. When all water was removed from the mixture, the product began slowly to crystallize. The obtained suspension was heated under reflux temperature for 1.5 h, then cooled and filtered. 2.75 g (88% from N,N-didesmethyl venlafaxine hydrochloride) of pure venlafaxine hydrochloride form I (HPLC: 99.65 area %) were obtained.

1. temperatureThe mixture was heated
2. customwater was removed by azeotropic distillation
3. customWhen all water was removed from the mixture
4. customto crystallize
5. temperatureThe obtained suspension was heated
6. temperatureunder reflux temperature for 1.5 h
7. temperaturecooled
8. filtrationfiltered