反应详情

To a stirred mixture of 2-bromo-4-fluorotrifluoromethylbenzene (33.7 g, 0.1387 mol) in sulfuric acid (98%, 34 mL) at 5° C. under nitrogen is added dropwise a mixture of sulfuric acid (98%, 10.1 mL) with fuming nitric acid (6.7 mL). The mixture is warmed up to room temperature for 2 hours and cooled down to 5° C. before adding water (60 mL). The resulting mixture is extracted twice with ethyl acetate (10 mL). The combined organic phases are washed with a saturated solution of sodium hydrogencarbonate (60 mL), water (60 mL) and dried over sodium sulfate. Concentration affords the title compound as a yellow solid (37.1 g, 92.9%)

1. additionis added dropwise
2. temperaturecooled down to 5° C.
3. extractionThe resulting mixture is extracted twice with ethyl acetate (10 mL)
4. washThe combined organic phases are washed with a saturated solution of sodium hydrogencarbonate (60 mL), water (60 mL)
5. dry with materialdried over sodium sulfate
6. concentrationConcentration