反应详情

To a solution of 1.00 g (1.13 mmol) of (5S)-2-(1-{5-[(tert-Butyldimethylsilyl)oxy]pyrimidin-2-yl}piperidin-4-yl)-4-(4,4-difluorocyclohexyl)-3-{(S)-fluoro[4-(trifluoromethyl)phenyl]methyl}-5-[(4-methoxybenzyl)oxy]-7,7-dimethyl-5,6,7,8-tetrahydroquinoline, which was prepared by a method similar to that of Reference Example 13, in 2 ml of tetrahydrofuran, 1.5 ml of a solution of 1.0 M tetra-n-butylammonium fluoride in tetrahydrofuran was added, and the reaction mixture was stirred at room temperature for 2 hours. After completion of the reaction, toluene and water were added to the reaction solution to separate an organic phase. Further, the reaction mixture was extracted with toluene from the aqueous phase. The obtained organic phases were combined and washed with saturated sodium chloride aqueous solution, and then the solvent was distilled off under reduced pressure. The obtained residue was subjected to silica gel column chromatography [n-hexane/ethyl acetate=78/22-55/45 (V/V)] and the fraction including the desired compound was concentrated under reduced pressure to provide 861 mg of the title compound as a white solid (yield: 99%).

1. additionwere added to the reaction solution
2. customto separate an organic phase
3. extractionFurther, the reaction mixture was extracted with toluene from the aqueous phase
4. washwashed with saturated sodium chloride aqueous solution
5. distillationthe solvent was distilled off under reduced pressure
6. concentrationwas concentrated under reduced pressure