反应详情

m-Chloroperoxybenzoic acid (77%, 0.14 g, 0.62 mmol) in dichloromethane (10 mL) was added at 0° C. to a solution of 269c) (0.33 g, 0.77 mmol) in dichloromethane (40 mL) and the reaction mixture was stirred at room temperature for 3 h. The mixture was then washed successively with saturated sodium hydrogen carbonate solution (2×20 mL) and brine (1×30 mL), dried over sodium sulfate and evaporated. The residue was purified by flash column chromatography [silica gel; dichloromethane with 2% methanol]. White solid. Yield: 0.215 g (63% of theory)

1. washThe mixture was then washed successively with saturated sodium hydrogen carbonate solution (2×20 mL) and brine (1×30 mL)
2. dry with materialdried over sodium sulfate
3. customevaporated
4. customThe residue was purified by flash column chromatography [silica gel; dichloromethane with 2% methanol]