反应详情

温度

90 °C

To a mixture of 1-(2,6-difluoro-4-nitrophenyl)-4-methoxy-2-oxo-1,2-dihydropyridine-3-carbonitrile obtained in Step A (3.00 g), ammonium chloride (5.22 g), ethanol (48 mL) and water (12 mL) was added iron powder (2.18 g) at room temperature, and the reaction mixture was heated at 90° C. for 1 hr. The reaction mixture was cooled to room temperature, and slowly poured into saturated sodium hydrogen carbonate solution, and the mixture was extracted with a mixed solvent of tetrahydrofuran/ethyl acetate=3/1. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. To the residue was added isopropyl ether (10 mL), and the mixture was stirred for 15 min. The precipitate was collected by filtration to give the title compound (1.95 g).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionthe mixture was extracted with a mixed solvent of tetrahydrofuran/ethyl acetate=3/1
3. washThe extract was washed with saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customthe solvent was evaporated under reduced pressure
6. additionTo the residue was added isopropyl ether (10 mL)
7. filtrationThe precipitate was collected by filtration