反应详情

温度

80 °C

In a sealed tube a mixture of enantiomer E1 of 3-(3,4-difluorophenyl)pyrrolidin-3-ol (0.26 g, 1.3 mmol), acetonitrile (3 mL), potassium carbonate (0.269 g, 1.95 mmol) and iodoethane (0.20 g, 1.3 mmol) was heated under microwave irradiation at 80° C. for 25 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 washed with brine, dried (Na2SO4) and evaporated. Purification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 35:65 to 50:50) gave the title compound (0.117 g). [α]D=+19.4° (methanol). The amine was converted to the fumaric acid salt and recrystallized from methanol/diethyl ether/diisopropyl ether: M.p. 136-137° C.; MS m/z (relative intensity, 70 eV) 227 (M+, 10), 207, (19), 141 (20), 72 (42), 71 (bp).

1. extractionthe aqueous phase was extracted with ethyl acetate (2×50 mL)
2. washthe combined organic phase was washed with brine
3. dry with materialdried (Na2SO4)
4. customevaporated
5. customPurification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 35:65 to 50:50)