HRID630550
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
m-Chloroperoxybenzoic acid (77%, 79 mg, 0.35 mmol) was added to an ice cooled solution of 341b) (0.2 g, 0.43 mmol) in dichloromethane (30 mL). The mixture was stirred at room temperature for 1 h and then diluted with dichloromethane (25 mL). The organic phase was washed successively with saturated sodium hydrogen solution (2×15 mL) and brine (1×15 mL), dried over sodium sulfate and evaporated. The residue was purified by flash column chromatography [silica; dichloromethane with 0-2% methanol]. White solid. Yield: 0.08 g (39% of theory)
WORKUP
后处理
- washThe organic phase was washed successively with saturated sodium hydrogen solution (2×15 mL) and brine (1×15 mL)
- dry with materialdried over sodium sulfate
- customevaporated
- customThe residue was purified by flash column chromatography [silica; dichloromethane with 0-2% methanol]