反应详情

To a 3 liter round bottom flask was charged with 500 ml H2SO4. Fuming nitric acid was added (40 mL) and the mixture gently stirred. 2-Bromo-5-fluorobenzoic acid (60 g, 219 mmol) was added in 5 g portions over 90 minutes at 5-10° C. The mixture was stirred for 60 minutes at which time the reaction was completed. The mixture was poured into 1 liter of an ice/water mixture and extracted with EtOAc (3×600 mL). The combined organic extracts are dried (MgSO4) and concentrated under reduced pressure to give a yellow solid. The solid was suspended in hexanes and stirred for 30 minutes. The solid was collected on filter to provide 2-bromo-5-fluoro-3-nitrobenzoic acid as yellow solid (35 g, 49%).

1. stirringThe mixture was stirred for 60 minutes at which time the reaction
2. extractionextracted with EtOAc (3×600 mL)
3. dry with materialThe combined organic extracts are dried (MgSO4)
4. concentrationconcentrated under reduced pressure
5. customto give a yellow solid
6. stirringstirred for 30 minutes
7. customThe solid was collected
8. filtrationon filter