反应详情

To the crude (−)-2-{1-[5-(4-Ethoxycarbonylbutoxyl)pyrimidin-2-yl]piperidin-4-yl}-4-(4,4-difluorocyclohexyl)-3-{fluoro[4-(trifluoromethyl)phenyl]methyl}-7,7-dimethyl-5,6,7,8-tetrahydroquinolin-5-ol obtained in Example (23-1), 2 ml of tetrahydrofuran, 2 ml of ethanol and 1 ml (1.00 mmol) of 1 N sodium hydroxide aqueous solution were added, and the reaction solution was stirred at room temperature for 1 hour. After completion of the reaction, 1 N hydrochloric acid was poured into the reaction solution under ice cooling and the reaction solution was extracted with methylene chloride. The organic layer was washed with saturated sodium chloride aqueous solution and dried with anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The obtained residue was purified by high performance liquid chromatography [YMC-pack ODS-A; acetonitrile/aqueous solution of 0.1% acetic acid and 0.1% triethylamine=85/15 (V/V)] to provide 63 mg of the title compound as a white solid (yield in two steps: 64%).

1. additionwas poured into the reaction solution under ice cooling
2. extractionthe reaction solution was extracted with methylene chloride
3. washThe organic layer was washed with saturated sodium chloride aqueous solution
4. dry with materialdried with anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customThe obtained residue was purified by high performance liquid chromatography [YMC-pack ODS-A; acetonitrile/aqueous solution of 0.1% acetic acid and 0.1% triethylamine=85/15 (V/V)]