反应详情

Ammonium chloride (6.24 g, 117 mmol) and iron powder (4.34 g, 77.7 mmol) were added to a stirred mixture of (2-bromo-3-fluoro-6-nitrophenyl)methylamine (4.84 g, 19.4 mmol) in 3:1 methanol/water (320 mL) and the resultant mixture heated at reflux for 24 h. The solid material was removed by filtration and the filtrate concentrated to approximately ⅓ volume. This mixture was partitioned between DCM (3×) and water then the combined DCM extracts were dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by chromatography (SiO2, eluting with 0-5% methanol in DCM) to give title compound as an oil (1.99 g, 47%). LCMS (Method C): RT 2.37 min [M+H]+ 219.0, 221.0

1. temperatureat reflux for 24 h
2. customThe solid material was removed by filtration
3. concentrationthe filtrate concentrated to approximately ⅓ volume
4. customThis mixture was partitioned between DCM (3×) and water
5. dry with materialthe combined DCM extracts were dried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe resulting residue was purified by chromatography (SiO2, eluting with 0-5% methanol in DCM)