反应详情

To a suspension of N-(2-cyano-5-methylphenyl)-2-fluoro-6-methoxybenzamide (31.5 g, 111 mmol) in ethanol (626 mL) was added 6 M aqueous NaOH solution (205 mL). After 10 minutes, 30% aqueous H2O2 (60 mL) was added, forming a slurry. The reaction was heated to reflux for 18 h and cooled to room temperature. NaOH (22.2 g, 0.56 mol) and 30% aqueous H2O2 (26 mL) were added, and the reaction was heated to reflux for six hours. The reaction cooled to room temperature, 30% aqueous H2O2 (45 mL) was added, and the reaction was heated to reflux for 18 h. The reaction was cooled to room temperature, NaOH (10 g, 0.25 mol) and 30% aqueous H2O2 (70 mL) were added, and the reaction was heated to reflux for six hours. The reaction was cooled to room temperature and poured over ice (800 mL). The pH was adjusted to 3-4 by addition of conc. HCl solution, and the precipitated off-white solid was filtered and washed with water (3×40 mL). The solid was dried under vacuum to provide 2-(2-fluoro-6-methoxy-phenyl)-7-methyl-3H-quinazolin-4-one (28 g, 89%).

1. customforming a slurry
2. temperatureThe reaction was heated
3. temperatureto reflux for 18 h
4. temperaturethe reaction was heated
5. temperatureto reflux for six hours
6. temperatureThe reaction cooled to room temperature
7. temperaturethe reaction was heated
8. temperatureto reflux for 18 h
9. temperatureThe reaction was cooled to room temperature
10. temperaturethe reaction was heated
11. temperatureto reflux for six hours
12. temperatureThe reaction was cooled to room temperature
13. filtrationthe precipitated off-white solid was filtered
14. washwashed with water (3×40 mL)
15. customThe solid was dried under vacuum