反应详情

A mixture of 7.7 g (22.7 mmol) of the 6-(3-chloro-5-fluoro-4-trifluoromethylphenyl)-3-propyltetrahydro-2-pyrone, 13.2 g (113.6 mmol) of triethylsilane, and 50 ml of trifluoroacetic acid was stirred at room temperature for 1 hour. After termination of the reaction, 30 ml of water was added to the reaction solution and extracted with 50 ml of toluene. The organic layer thus obtained was washed with a diluted aqueous sodium bicarbonate solution thrice and water thrice, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under a reduced pressure and the residue was subjected to silica gel column chromatography (eluent: heptane/toluene=9/1) to obtain 6.6 g of a crude trans-2-(3-chloro-5-fluoro-4-trifluoromethylphenyl)-5-propyltetrahydropyran.

1. additionwas added to the reaction solution
2. extractionextracted with 50 ml of toluene
3. customThe organic layer thus obtained
4. washwas washed with a diluted aqueous sodium bicarbonate solution thrice and water thrice
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off under a reduced pressure