反应详情

温度

50 °C

To a solution of 183 mg (0.500 mmol) of ethyl 2,2-dimethyl-3-(1-acetoxy-2,2-dichloro-3,3,3-trifluoropropyl)cyclopropanecarboxylate obtained in Example 9, in 0.5 ml of DMF, 35 mg (0.54 mmol) of zinc powder was added, and the mixture was stirred at 50° C. for 4 hours. After an addition of 1 ml of a saturated ammonium chloride aqueous solution, the mixture was extracted with diethyl ether (1 ml×5 times). The extract was dried over anhydrous magnesium sulfate, then filtered and concentrated under reduced pressure. The product was purified by thin layer chromatography (silica gel, dichloromethane/hexane=1/3) to obtain 116 mg of ethyl 2,2-dimethyl-3-(2-chloro-3,3,3-trifluoro-1-propenyl)-cyclopropane carboxylate as a colorless oil.

1. extractionthe mixture was extracted with diethyl ether (1 ml×5 times)
2. dry with materialThe extract was dried over anhydrous magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe product was purified by thin layer chromatography (silica gel, dichloromethane/hexane=1/3)