反应详情

温度

90 °C

To a mixture of (2-bromo-3-fluoro-6-nitrophenyl)phenylamine (2.4 g, 7.7 mmol) in MeOH (40 mL) and water (15 mL) were added NH4Cl (2.38 g, 46.3 mmol) and iron powder (1.72 g, 30.9 mmol) and the reaction mixture heated at 90° C. for 1 h. After cooling to RT, the crude mixture was filtered through a pad of Celite® and the filtrate concentrated in vacuo. The resulting residue was partitioned between EtOAc and water. The aqueous phase was extracted with EtOAc (×3) and the combined organic fractions washed with brine, dried (MgSO4) and concentrated in vacuo to afford the title compound (1.95 g, 90%). LCMS (Method C): RT 3.48 min [M+H]+ 281.1/283.1.

1. temperatureAfter cooling to RT
2. filtrationthe crude mixture was filtered through a pad of Celite®
3. concentrationthe filtrate concentrated in vacuo
4. customThe resulting residue was partitioned between EtOAc and water
5. extractionThe aqueous phase was extracted with EtOAc (×3)
6. washthe combined organic fractions washed with brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated in vacuo