HRID1242501

反应详情

EQUATION

反应方程式

HRID 1242501 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.0 g (11.2 mmol) of 2-(4-acetyl-3-fluoro-phenoxy)-2-methyl-propionic acid ethyl ester in 30 ml dichloromethane was treated with 4.1 g (70%, 16.8 mmol) of 3-chloro perbenzoic acid. The reaction was stirred at RT. After 1 day additional 1.2 g (70%, 4.7 mmol), after 2 days 0.8 g (70%, 3.1 mmol) and after 3 days 0.6 g (70%, 2.3 mmol) of 3-chloro perbenzoic acid were added. The mixture was poured on ice/aqueous 10% disodium pyroslfite solution and extracted with ether (3×). The organic phases were washed with aqueous 10% NaHCO3, aqueous saturated NH4Cl, aqueous 10% NaCl and dried over sodium sulfate to give 3.2 g of the title compound as light yellow oil.

WORKUP

后处理

  1. waitafter 2 days 0.8 g (70%, 3.1 mmol)
  2. additionThe mixture was poured on ice/aqueous 10% disodium pyroslfite solution
  3. extractionextracted with ether (3×)
  4. washThe organic phases were washed with aqueous 10% NaHCO3, aqueous saturated NH4Cl, aqueous 10% NaCl
  5. dry with materialdried over sodium sulfate