反应详情

m-Chloroperoxybenzoic acid (77%, 0.20 g, 0.92 mmol) in THF (5 mL) was added to an ice-cooled solution of 223c) (0.54 g, 1.02 mmol) in THF (100 mL) and the resulting mixture was stirred at room temperature for 4 h. The reaction mixture was then diluted with ethyl acetate (50 mL) and successively washed with saturated sodium hydrogen carbonate solution (2×50 mL) and brine (1×50 mL). The organic phase was dried over sodium sulfate and evaporated. The residue was purified by flash column chromatography [silica gel; dichloromethane with 2% methanol]. White solid. Yield: 0.28 g (51% of theory)

1. washsuccessively washed with saturated sodium hydrogen carbonate solution (2×50 mL) and brine (1×50 mL)
2. dry with materialThe organic phase was dried over sodium sulfate
3. customevaporated
4. customThe residue was purified by flash column chromatography [silica gel; dichloromethane with 2% methanol]