反应详情

26 g of 1-benzyloxy-9,9,10,10,10-pentafluoro-decane is dissolved in 1000 ml of absolute methylene chloride, mixed with 28.9 ml of N,N-dimethylaniline at 0° C. and stirred for 5 minutes. Then, 41.1 g of aluminum trichloride is added in portions, and the reaction mixture is heated for 45 minutes to 50° C. For working-up, the batch is allowed to come to room temperature, it is stirred into 2N hydrochloric acid, extracted 3 times with methylene chloride, the organic phase is washed with common salt solution, dried on magnesium sulfate and concentrated by evaporation in a vacuum. The crude product is chromatographed on silica gel with a hexane-ethyl acetate gradient. 7.8 g of 9,9,10,10,10-pentafluoro-decan-1-ol is obtained as an oil.

1. temperaturethe reaction mixture is heated for 45 minutes to 50° C
2. customto come to room temperature
3. extractionextracted 3 times with methylene chloride
4. washthe organic phase is washed with common salt solution
5. customdried on magnesium sulfate
6. concentrationconcentrated by evaporation in a vacuum
7. customThe crude product is chromatographed on silica gel with a hexane-ethyl acetate gradient