反应详情

温度

60 °C

To a solution of 1-cyclopropyl-6,7-difluoro-1H-quinazoline-2,4-dione (Example 23a, 2.0 g, 8.92 mmol) in dioxane (7.5 mL) and dimethylformamide (7.5 mL) is added NaH (60% dispersion in oil, 428 mg, 10.7 mmol). The solution is heated to 60° C. for 10 minutes and cooled to room temperature. To the cooled solution is added O-(2,4-dinitrophenyl)hydroxylamine (1.77 g, 8.92 mmol), and the solution is heated to 80° C. for 30 minutes. The resulting red solution is cooled to room temperature, poured over crushed ice, and extracted with EtOAc. The combined organic layers are dried over MgSO4, filtered, and the solvent removed under reduced pressure. The resulting solid is triturated with Et2O and air dried to afford 1.44 g of the title compound. MS CI: m/z 254 (MH+).

1. temperaturecooled to room temperature
2. temperaturethe solution is heated to 80° C. for 30 minutes
3. temperatureThe resulting red solution is cooled to room temperature
4. additionpoured
5. customover crushed ice
6. extractionextracted with EtOAc
7. dry with materialThe combined organic layers are dried over MgSO4
8. filtrationfiltered
9. customthe solvent removed under reduced pressure
10. customThe resulting solid is triturated with Et2O and air
11. customdried