反应详情

To a solution of 1-bromo-2,4-difluoro-5-nitrobenzene (5.04 g, 21.3 mmol) in EtOH (100 mL), THF (50 mL), NH4Cl (sat) (25 mL) and H2O (25 mL) was added iron powder (5.0 g, 89.5 mmol). The mixture was refluxed for 2 h and filtered through celite. The filter pad was washed with EtOAc (3×50 mL). The filtrate was concentrated and the residue was partitioned between EtOAc and brine. The organic layer was dried over MgSO4 and concentrated. Purification by flash chromatography (5–10% EtOAc/Hexane) provided 2.6 g (59%) of 5-bromo-2,4-difluoroaniline: ESMS m/e: 208.2 (M+H)+.

1. temperatureThe mixture was refluxed for 2 h
2. filtrationfiltered through celite
3. washThe filter pad was washed with EtOAc (3×50 mL)
4. concentrationThe filtrate was concentrated
5. customthe residue was partitioned between EtOAc and brine
6. dry with materialThe organic layer was dried over MgSO4
7. concentrationconcentrated
8. customPurification by flash chromatography (5–10% EtOAc/Hexane)