反应详情

m-Chloroperoxybenzoic acid (0.114 g, 0.66 mmol, 0.9 eq) was added at 0° C. to a stirred solution of 244c) (0.400 g, 0.61 mmol, 1 eq) in dichloromethane (30 mL). The reaction mixture was stirred for 3 h at room temperature, then diluted with dichloromethane (50 mL) and successively washed with saturated sodium hydrogen carbonate solution (2×30 mL) and brine (30 mL). The organic layer wasdried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography [230-400 mesh silica gel, dichloromethane/methanol=95:5]. White solid. Yield: 0.290 g (71% of theory)

1. washsuccessively washed with saturated sodium hydrogen carbonate solution (2×30 mL) and brine (30 mL)
2. concentrationconcentrated under reduced pressure
3. customThe residue was purified by column chromatography [230-400 mesh silica gel, dichloromethane/methanol=95:5]