反应详情

3.2 g of 98 in 50 ml of methylene chloride/methanol 1:1 is dissolved, and 750 mg of p-toluenesulfonic acid is added. It is stirred under argon for 2 hours at room temperature. Sodium chloride solution is added, extracted with methylene chloride, the organic phase is washed with sodium bicarbonate solution and sodium chloride solution, dried on sodium sulfate and concentrated by evaporation. The residue is chromatographed on silica gel with ethyl acetate/hexane, whereby 2.7 g of 1-[1-(1-hydroxy-2,2,3,3,4,4,5,5,5-nonafluoropentyl)cyclopropyl]ethanone 99 is obtained as a colorless oil.

1. extractionextracted with methylene chloride
2. washthe organic phase is washed with sodium bicarbonate solution and sodium chloride solution
3. customdried on sodium sulfate
4. concentrationconcentrated by evaporation
5. customThe residue is chromatographed on silica gel with ethyl acetate/hexane