反应详情

To a stirred mixture of 5.0 g (0.017 mole) of 1-(4-chloro-2-fluoro-5-hydroxyphenyl)-4-difluoromethyl-4,5-dihydro-3-methyl-1,2,4-triazol-5(1H)-one and 2.6 g (0.019 mole) of potassium carbonate in 25 mL of acetone was added 2.7 g (0.017 mole) of 2-chloro-5-nitropyridine. The mixture was stirred at room temperature for one hour, then was heated at reflux for two hours. The mixture was allowed to cool to room temperature and was stirred for approximately 18 hours. The reaction mixture was heated at reflux for an additional four hours, then cooled and stirred at room temperature for approximately 18 hours. The mixture was filtered, and the filtrate was evaporated under reduced pressure to leave an oily residue, which crystallized upon standing to give 7.0 g of 1-[4-chloro-2-fluoro-5-(5-nitropyridin-2-yloxy)phenyl]-4-difluoromethyl -4,5-dihydro-3-methyl-1,2,4-triazol-5(1H)-one, m.p. 120°-123° C.

1. temperaturewas heated
2. temperatureat reflux for two hours
3. temperatureto cool to room temperature
4. stirringwas stirred for approximately 18 hours
5. temperatureThe reaction mixture was heated
6. temperatureat reflux for an additional four hours
7. temperaturecooled
8. stirringstirred at room temperature for approximately 18 hours
9. filtrationThe mixture was filtered
10. customthe filtrate was evaporated under reduced pressure
11. customto leave an oily residue, which
12. customcrystallized