反应详情

To a solution of 4-nitroaniline (50 g, 0.36 mol) in AcOH (500 mL) was added liquid Br2 (60 g, 0.38 mol) dropwise at 5 CC. The mixture was stirred for 30 min at that temperature. The insoluble solid was collected by filtration and poured into EtOAc (200 mL). The mixture was basified with saturated aqueous NaHCO3 to pH 7. The organic layer was separated. The aqueous phase was extracted with EtOAc (300 mL×3). The combined organic layers were dried and evaporated under reduced pressure to give 2-bromo-4-nitroaniline (56 g, 72%), which was directly used in the next step.

1. filtrationThe insoluble solid was collected by filtration
2. additionpoured into EtOAc (200 mL)
3. customThe organic layer was separated
4. extractionThe aqueous phase was extracted with EtOAc (300 mL×3)
5. customThe combined organic layers were dried
6. customevaporated under reduced pressure