反应详情

Add zinc (4.0 g) to a solution of 6-chloro-3-nitropyridin-2-yl-amine (1.0 g, 5.76 mmol) in acetic acid (1.5 mL) and methanol (40 mL). Stir the resulting mixture is at room temperature for 18 hours, and filter through a pad of celite. Evaporate the filtrate to dryness under reduced pressure. Treat the resulting residue with 1N aqueous NaOH and extract with EtOAc. Wash the EtOAc extract with water and saturated aqueous NaCl. Separate the organic layer, dry over Na2SO4, filter and concentrate. Purify by flash column chromatography (50% EtOAc-hexane) to obtain 6-chloro-pyridine-2,3-diamine.

1. filtrationfilter through a pad of celite
2. customEvaporate the filtrate to dryness under reduced pressure
3. additionTreat the resulting residue with 1N aqueous NaOH
4. extractionextract with EtOAc
5. washWash the EtOAc
6. extractionextract with water and saturated aqueous NaCl
7. customSeparate the organic layer
8. dry with materialdry over Na2SO4
9. filtrationfilter
10. concentrationconcentrate
11. customPurify by flash column chromatography (50% EtOAc-hexane)