反应详情

To a solution of 135 mg (0.794 mmol) of ethyl 2,2-dimethyl-3-(1-hydroxy-2,2-dichloro-3,3,3-trifluoropropyl)cyclopropanecarboxylate obtained in Example 2, in 2 ml of diethyl ether, 0.073 ml (0.94 mmol) of methanesulfonyl chloride and 0.133 ml (0.95 mmol) of triethylamine, were added, and the mixture was stirred at room temperature for 2 hours. After an addition of 5 ml of hexane to the mixture, the precipitated inorganic salt was 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 157 mg of ethyl 2,2-dimethyl-3-(1-methanesulfonyloxy-2,2-dichloro-3,3,3trifluoropropyl)cyclopropanecarboxylate as a colorless oily substance.

1. filtrationthe precipitated inorganic salt was filtered off
2. concentrationthe filtrate was concentrated under reduced pressure
3. customThe product was purified by thin layer chromatography (silica gel, dichloromethane/hexane=1/1)