HRID1607361

反应详情

EQUATION

反应方程式

HRID 1607361 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 390 mg (0.821 mmol) of (2-methyl-3-phenylphenyl)methyl 2,2-dimethyl-3-(1-hydroxy-2,2-dichloro-3,3,3-trifluoropropyl)cyclopropanecarboxylate obtained in Example 3, in 2 ml of diethyl ether, 0.114 ml (0.98 mmol) of benzoyl chloride and 0.137 ml of triethylamine, were added, and the mixture was stirred at room temperature for 12 hours. Then, 0.23 ml of benzoyl chloride and 0.28 ml of triethylamine were further added, and the mixture was stirred overnight at room temperature. After an addition of 5 ml of hexane, the inorganic salts are filtered off, and the filtrate was concentrated under reduced pressure. The product was purified by thin layer chromatography (silica gel, dichloromethane/hexane=1/1) to obtain 175 mg of (2-methyl-3-phenylphenyl)methyl 2,2-dimethyl-3-(1-benzoyloxy-2,2-dichloro-3,3,3-trifluoropropyl)cyclopropanecarboxylate as a colorless oily substance.

WORKUP

后处理

  1. stirringthe mixture was stirred overnight at room temperature
  2. filtrationthe inorganic salts are filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe product was purified by thin layer chromatography (silica gel, dichloromethane/hexane=1/1)