反应详情

温度

100 °C

A suspension of 1-benzhydrylazetidin-3-yl methanesulfonate (247 mg, 0.78 mmol) in trifluoropropanol (1 g, 7.8 mmol) was placed under micro-wave irradiations (100 W) and heated at 100° C. during 30 minutes. The reaction mixture was diluted by addition of dichloromethane (50 mL) and water (30 mL). The two phases were separated and the aqueous phase was extracted with dichloromethane (2×20 mL). The combined organic phases were dried over sodium sulphate and concentrated to dryness. The residue was purified by chromatography on silica gel using petroleum ether/ethyl acetate (8:2) as eluent. The title product was isolated as a yellow oil (191 mg, 33%).

1. customThe two phases were separated
2. extractionthe aqueous phase was extracted with dichloromethane (2×20 mL)
3. dry with materialThe combined organic phases were dried over sodium sulphate
4. concentrationconcentrated to dryness
5. customThe residue was purified by chromatography on silica gel