Reaktion #42025

Reaktionsgleichung

venlafaxine

isopropyl acetate

HCl

→

venlafaxine hydrochloride

Ausbeute 88.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated
2. 2
   Sonstigewater was removed by azeotropic distillation
3. 3
   SonstigeWhen all water was removed from the mixture
4. 4
   Sonstigeto crystallize
5. 5
   TemperaturThe obtained suspension was heated
6. 6
   Temperaturunder reflux temperature for 1.5 h
7. 7
   Temperaturcooled
8. 8
   Filtrationfiltered

Vorschrift

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.

Quelle