反应详情

Ethyl 6-{3-[3,5-bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}-2-(trifluoro-methyl)nicotinate (1.7 g) was added to dichloromethane (50 ml). Then, 1.0 mol/l hexane solution (10 ml) of diisobutyl aluminum hydride was added dropwise thereto at −70° C. After continuing the stirring at −70° C. for 30 minutes, ethyl acetate (50 ml) and sodium sulfate decahydrate (3.0 g) were added. After further stirring at room temperature for 1 hour, the reaction liquid was filtered by suction on Celite. The filtrate was distilled off under reduced pressure and the purified by silica gel column chromatography to obtain [6-{3-[3,5-bis-(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}-2-(trifluoromethyl)pyridin-3-yl]-methanol (1.55 g).

1. customat −70° C
2. customstirring at −70° C.
3. customfor 30 minutes
4. customthe reaction liquid
5. filtrationwas filtered by suction on Celite
6. distillationThe filtrate was distilled off under reduced pressure
7. customthe purified by silica gel column chromatography