反应详情

To a solution of 406 mg (0.855 mmol) of (2-methyl-3phenylphenyl)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, 0.079 ml (1.0 mmol) of methanesulfonyl chloride and 0.143 ml (1.0 mmol) of triethylamine, were added, and the mixture was stirred at room temperature for 1 hour. 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 458 mg of (2-methyl-3-phenylphenyl)methyl 2,2-dimethyl-3-(1-methanesulfonyloxy-2,2-dichloro-3,3,3-trifluoropropyl)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)