反应详情

温度

40 °C

2,4-Dichloro-3-nitropyridine c (2.058 g, 10.7 mmol) was dissolved in HOAc (10 mL) under nitrogen. Iron powder (1.9191 g, 34.4 mmol) was added. The sample was heated at 40° C. for two hours. The reaction mixture was poured onto ice and then NaHCO3 was added to give a neutral solution. The sample was extracted with EtOAc (3×100 mL). The EtOAc extracts were washed with saturated NaHCO3 (1×100 mL). The combined aqueous layers were back extracted once with 100 mL EtOAc. The combined EtOAc extracts were dried over MgSO4, filtered, and concentrated to give 3-amino-2-4-dichloropyridine d (1.510 g, 9.26 mmol, 87%).

1. additionThe reaction mixture was poured onto ice
2. customto give a neutral solution
3. extractionThe sample was extracted with EtOAc (3×100 mL)
4. washThe EtOAc extracts were washed with saturated NaHCO3 (1×100 mL)
5. extractionThe combined aqueous layers were back extracted once with 100 mL EtOAc
6. dry with materialThe combined EtOAc extracts were dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated