HRID851380

反应详情

EQUATION

反应方程式

HRID 851380 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of benzyl 4-[(2RS)-4-oxoazetidin-2-yl]but-2-enoate (167 mg), tert-butylhydroperoxide (0.3 ml), and sodium tetrachloropalladate (80 mg) in 67% aqueous acetic acid (2.7 ml) was heated at 50° C. for 8.5 hours. Additional tert-butylhydroperoxide (0.5 ml) and sodium tetrachloropalladate (40 mg) were added. The reaction mixture was stirred at room temperature for three days and heated at 50° C. for 14 hours. After evaporation of the solvent in vacuo, the residue was taken up into ethyl acetate (20 ml) and washed with dilute aqueous sodium chloride. Drying over magnesium sulfate and evaporation left an oil (200 mg), which was chromatographed on silica gel plate (developing solvent: 20% acetone in dichloromethane) afforded benzyl 3-oxo-4-[(2RS)-4-oxoazetidin-2-yl]butanoate (66 mg).

WORKUP

后处理

  1. temperatureheated at 50° C. for 14 hours
  2. customAfter evaporation of the solvent in vacuo
  3. washwashed with dilute aqueous sodium chloride
  4. dry with materialDrying over magnesium sulfate and evaporation
  5. waitleft an oil (200 mg), which
  6. customwas chromatographed on silica gel plate (developing solvent: 20% acetone in dichloromethane)