反应详情

Sodium hydride (60% in oil, 2.12 g) wad added to an N,N-dimethylformamide solution (100 ml) of 4-trifluoromethoxyphenol (9.0 g) under ice cooling and stirred for 30 minutes. After adding 4-[2-(toluene-4-sulfonyloxy)ethyl]piperidine-1-carboxylic acid tert-butyl ester (17.7 g), the mixture was heated to room temperature and stirred. The mixture was further stirred at 50° C. for 1 hour. After cooling the reaction mixture to room temperature, water was added thereto, followed by extraction with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution and dried over sodium sulfate. The result was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=67:33) to afford the title compound as a pale yellow oil (18.64 g).

1. stirringstirred
2. stirringThe mixture was further stirred at 50° C. for 1 hour
3. temperatureAfter cooling the reaction mixture to room temperature
4. extractionfollowed by extraction with ethyl acetate
5. washThe organic layer was washed with a saturated sodium chloride aqueous solution
6. dry with materialdried over sodium sulfate
7. concentrationThe result was concentrated under reduced pressure
8. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=67:33)