HRID630550

反应详情

EQUATION

反应方程式

HRID 630550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washThe organic phase was washed successively with saturated sodium hydrogen solution (2×15 mL) and brine (1×15 mL)
  2. dry with materialdried over sodium sulfate
  3. customevaporated
  4. customThe residue was purified by flash column chromatography [silica; dichloromethane with 0-2% methanol]