反应详情

To a solution of 10 g 1-(4-Nitro-phenyl)-1H-pyridin-4-one in 510 mL ethyl acetate and 26 mL ethanol, 52.1 g SnCl2 dihydrate were added and the reaction mixture was heated to reflux for 6 h. Then, after cooling to RT the solvents were removed under reduced pressure. The residue was taken-up in 100 mL aqueous NaHCO3 solution and 200 mL ethyl acetate were added. The inorganic precipitate was filtered off and the solids were washed with ethyl acetate. After separation of the organic layer, the aqueous layer of the filtrate was extracted with ethyl acetate (2×100 ml) and with DCM (3×150 ml). The combined organic layers were dried over Na2SO4 and the solvents were removed under reduced pressure. The remaining product was pure enough for the next reaction step. Yield: 6 g.

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 6 h
3. customwere removed under reduced pressure
4. addition200 mL ethyl acetate were added
5. filtrationThe inorganic precipitate was filtered off
6. washthe solids were washed with ethyl acetate
7. customAfter separation of the organic layer
8. extractionthe aqueous layer of the filtrate was extracted with ethyl acetate (2×100 ml) and with DCM (3×150 ml)
9. dry with materialThe combined organic layers were dried over Na2SO4
10. customthe solvents were removed under reduced pressure
11. customThe remaining product was pure enough for the next reaction step