反应详情

To H2SO4 (98%, 15 ml) was added 6-bromo-7-methylquinazolin-4(3H)-one (1.0 g, 4.2 mmol) and the mixture was stirred at rt 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 rt 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 concentated in vacuo. The product was recrystalized from MeOH (˜15 ml). MS (M+H)+ 284, 286.

1. temperatureThe mixture was cooled to 0° C.
2. stirringstirred for 10 min
3. stirringstirred at rt for 5 h
4. additionThe mixture was poured onto ice (300 g)
5. extractionextracted with EtOAc (3×80 ml)
6. washThe combined organic layers were washed with brine (100 ml)
7. dry with materialdried over MgSO4
8. customThe product was recrystalized from MeOH (˜15 ml)