反应详情

A solution of 1-benzhydrylazetidin-3-yl methanesulfonate (500 mg, 1.57 mmol) in trifluoroethanol (3.5 mL, 30.7 mmol) was stirred under microwaves at 110° C. for 30 minutes. The reaction mixture was diluted by addition of dichloromethane (100 mL) and a saturated solution of sodium hydrogencarbonate (25 mL). The aqueous layer was separated and extracted with dichloromethane (2×10 mL). The combined organic phase was dried over sodium sulfate, filtered and concentrated to dryness. The residue was purified by chromatography on silica gel using dichloromethane/ethyl acetate (90:10) as eluent. The title product was obtained as a light yellow gum (170 mg, 32%).

1. customThe aqueous layer was separated
2. extractionextracted with dichloromethane (2×10 mL)
3. dry with materialThe combined organic phase was dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated to dryness
6. customThe residue was purified by chromatography on silica gel