反应详情

温度

120 °C

In a sealed tube a mixture of 3-(3-chloro-2-fluorophenyl)pyrrolidin-3-ol (0.5 g, 2.32 mmol), acetonitrile (3 mL), potassium carbonate (0.48 g, 3.48 mmol) and iodoethane (0.36 g, 2.32 mmol) was heated under microwave irradiation at 120° C. for 20 minutes. Aqueous sodium carbonate (10%, 50 mL) was added and the aqueous phase was extracted with ethyl acetate (2×50 mL). The combined organic phase was dried (Na2SO4) and evaporated. Purification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 20:80 to 50:50) gave the title compound. The amine was converted to the fumaric acid salt and recrystallized from methanol/diethyl ether/diisopropyl ether (0.249 g). M.p. 142-145.5° C.; MS m/z (relative intensity, 70 eV) 243 (M+, 24), 228 (19), 157 (15), 72 (27), 71 (bp).

1. extractionthe aqueous phase was extracted with ethyl acetate (2×50 mL)
2. dry with materialThe combined organic phase was dried (Na2SO4)
3. customevaporated
4. customPurification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 20:80 to 50:50)