反应详情

温度

90 °C

To a solution of 1,2-difluoro-4-nitrobenzene (2.94 g, 18.45 mmol) in DMF (30 mL) were added Et3N (3.11 g, 30.75 mmol) and bis(2-propoxyethyl)amine (1.16 g, 6.15 mmol) with stirring. The reaction mixture was heated at 90° C. overnight, then cooled to rt and poured into CH2Cl2 (100 mL). The organic phase was washed with water (100 mL×3), 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 yellow oil (1.47 g, 73%).

1. temperaturecooled to rt
2. washThe organic phase was washed with water (100 mL×3)
3. dry with materialdried over anhydrous Na2SO4
4. concentrationconcentrated in vacuo
5. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=10:1)