反应详情

温度

80 °C

To a mixture of (5-fluoro-2-nitro-phenyl)-pyridin-4-yl-amine (375 mg, 1.61 mmol) in a 3:1 mixture of MeOH:water (40 mL) were added NH4Cl (516 mg, 9.65 mmol) and iron powder (359 mg, 6.43 mmol) and the reaction mixture heated at 80° C. for 2 h. After cooling to RT, the solid was filtered through a pad of Celite® and washed with additional MeOH. The filtrate was concentrated in vacuo and the resulting residue partitioned between DCM and a saturated aqueous solution of NaHCO3. The organic fraction was dried and concentrated in vacuo to afford the title compound as a dark beige solid (215 mg, 66%). LCMS (Method C): RT 1.32 min [M+H]+ 204.09

1. temperatureAfter cooling to RT
2. filtrationthe solid was filtered through a pad of Celite®
3. washwashed with additional MeOH
4. concentrationThe filtrate was concentrated in vacuo
5. customthe resulting residue partitioned between DCM
6. customThe organic fraction was dried
7. concentrationconcentrated in vacuo