反应详情

温度

90 °C

To a solution of 3,4-difluoronitrobenzene (1.59 g, 10 mmol) in DMSO (15 mL) were added K2CO3 (3.04 g, 22 mmol) and diisobutylamine (1.42 g, 11 mmol). The mixture was heated at 90° C. overnight, then cooled to rt, diluted with water (50 mL) and extracted with CH2Cl2 (50 mL×3). The combined organic phases were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=10:1) to give the title compound as pale yellow oil (0.80 g, 30%).

1. temperaturecooled to rt
2. extractionextracted with CH2Cl2 (50 mL×3)
3. dry with materialThe combined organic phases were dried over anhydrous Na2SO4
4. concentrationconcentrated in vacuo
5. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=10:1)