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0 °C

6-Bromo-7-methylquinazolin-4(3H)-one (1.0 g, 4.2 mmol) was added to H2SO4 (98%, 15 mL) and the mixture was stirred at it until dissolution was complete. The mixture was cooled to 0° C. and then nitric acid (fuming) (0.26 g, 4.2 mmol) was added dropwise at 0° C. and stirred for 10 min, and then stirred at it for 5 h. The mixture was poured onto ice (300 g) and extracted with EtOAc (3×80 mL). The combined organic layers were washed with brine (100 mL), dried over MgSO4 and concentrated in vacuo. The product was recrystallized from MeOH (˜15 mL). MS (ESI, pos. ion) m/z: 284 [M+H]+

1. stirringstirred for 10 min
2. stirringstirred at it for 5 h
3. additionThe mixture was poured onto ice (300 g)
4. extractionextracted with EtOAc (3×80 mL)
5. washThe combined organic layers were washed with brine (100 mL)
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo
8. customThe product was recrystallized from MeOH (˜15 mL)