反应详情

温度

90 °C

To a solution of 3,4-difluoronitrobenzene (3.18 g, 20 mmol) in DMSO (25 mL) were added K2CO3 (6.08 g, 44 mmol) and di-n-butylamine (2.84 g, 22 mmol) with stirring. The mixture was heated at 90° C. overnight, then cooled to rt, diluted with water (100 mL) and extracted with CH2Cl2 (80 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/CH2Cl2 (V/V)=10:1) to give the title compound as yellow oil (4.03 g, 75%).

1. temperaturecooled to rt
2. extractionextracted with CH2Cl2 (80 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/CH2Cl2 (V/V)=10:1)