Hexane → Ethyl 2,2-dimethyl-3-(1-methanesulfonyloxy-2,2-dichloro-3,3,3trifluoropropyl)cyclopropanecarboxylate

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Reaction Steps

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.

Provenance & Evidence