反应详情

温度

120 °C

A mixture of 3-(3-chloro-5-fluorophenyl)azetidin-3-ol (0.41 g, 2.03 mmol), potassium carbonate (0.56 g, 4.06 mmol) and iodoethane (0.31 g, 2.03 mmol) in acetonitrile (5 ml) was heated at 120° C. under microwave irradiation for 10 min. Water (50 ml) and ethyl acetate (50 ml) was added and the organic phase was collected. The aqueous phase was extracted with ethyl acetate (2×50 ml). The combined organic phase was dried (Na2SO4) and evaporated under reduced pressure to give the crude product. Purification by flash column chromatography on silica gel (ethyl acetate) gave 0.28 g (60%) of the title compound. The amine was converted to the fumaric acid salt and recrystallized from ethanol/diethyl ether/diisopropyl ether: M.p. 166-168° C. MS m/z (relative intensity, 70 eV) 229 (M+, 1), 172 (23), 130 (24), 109 (33), 58 (bp).

1. customthe organic phase was collected
2. extractionThe aqueous phase was extracted with ethyl acetate (2×50 ml)
3. dry with materialThe combined organic phase was dried (Na2SO4)
4. customevaporated under reduced pressure
5. customto give the crude product
6. customPurification by flash column chromatography on silica gel (ethyl acetate)