反应详情

The solution of tert-butyl 6-chloro-4-iodopyridin-3-ylcarbamate (10.0 g, 28 mmol) in 3M HCl (600 mL) was heated at 60° C. for 12 h. The mixture was allowed to cool to room temperature and treated with sat. NaHCO3 to pH=8. The aqueous layer was extracted with ethyl acetate (100 mL×3). The combined organic layers were washed with brine, dried over anhydrous Na2SO4, concentrated and purified by chromatography on silica gel (10% ethyl acetate in petroleum ether as eluant) to afford 6-chloro-4-iodopyridin-3-amine (6.6 g, 93%). 1H-NMR (CDCl3, 400 MHz) δ 7.81 (s, 1H), 7.60 (s, 1H), 4.13 (br s, 2H).

1. extractionThe aqueous layer was extracted with ethyl acetate (100 mL×3)
2. washThe combined organic layers were washed with brine
3. dry with materialdried over anhydrous Na2SO4
4. concentrationconcentrated
5. custompurified by chromatography on silica gel (10% ethyl acetate in petroleum ether as eluant)