反应详情

Preparation according to Example 2: 3-(3-chloro-4-fluorophenyl)pyrrolidin-3-ol (0.31 g, 1.46 mmol), acetonitrile (3 mL), potassium carbonate (0.20 g, 1.46 mmol), iodoethane (0.12 mL, 1.5 mmol). Microwave irradiation at 100° C. for 20 minutes. Purification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 55:45). Yield: 0.19 g. The amine was converted to the fumaric acid salt and recrystallized from ethanol/diethyl ether/diisopropyl ether: M.p. 157-158° C.; MS m/z (relative intensity, 70 eV) 243 (M+, 9), 228 (9), 157 (13), 129 (10), 71 (bp).

1. customPreparation
2. customMicrowave irradiation at 100° C. for 20 minutes
3. customPurification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 55:45)
4. customrecrystallized from ethanol/diethyl ether/diisopropyl ether