反应详情

Preparation according to Example 8: 3-(3,4-difluorophenyl)pyrrolidin-3-ol (0.38 g, 1.9 mmol), acetonitrile (20 mL), sodium carbonate (0.26 g, 4.75 mmol), iodoethane (0.29 g, 1.9 mmol). Refluxed 2 h. Purification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 35:65 to 50:50). Yield: 0.26 g. The amine was converted to the fumaric acid salt and recrystallized from 2-propanol/diisopropyl ester: M.p. 157-158° C.; MS m/z (relative intensity, 70 eV) 227 (M+, 26), 212 (18), 141 (30), 127 (23), 113 (22), 71 (bp).

1. customPreparation
2. temperatureRefluxed 2 h
3. customPurification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 35:65 to 50:50)
4. customrecrystallized from 2-propanol/diisopropyl ester