反应详情

Toluene-4-sulfonic acid 4-(2-chloro-4-nitroimidazol-1-yl)-2-hydroxy-butyl ester (0.78 g) was suspended in ethanol (12 ml), an ethanol solution (0.68 ml) of 20% sodium ethoxide was added thereto, followed by stirring at room temperature for 1 hour. 4-[4-(4-Trifluoromethoxyphenoxy)piperidin-1-yl]phenol (0.707 g) and tripotassium phosphate (0.509 g) were added thereto and stirred at 80° C. for 2 hours. The mixture was cooled to room temperature and filtered through Celite to remove insoluble matter and, then the residue was washed with ethyl acetate. The filtrate and liquid were combined and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:1→9:1) to afford the title compound as a pale yellow powder (0.314 g).

1. stirringstirred at 80° C. for 2 hours
2. temperatureThe mixture was cooled to room temperature
3. filtrationfiltered through Celite
4. customto remove insoluble matter
5. washthe residue was washed with ethyl acetate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:1→9:1)