反应详情

A mixture of 0.379 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine, 0.21 g of imidazole and 15 ml of chloroform was heated under reflux for 8 hours. After the reaction mixture was concentrated, the residue was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over sodium sulfate. After the solvent was distilled off, 5 ml of acetic acid and 0.5 g of reduced iron were added to the residue, and the mixture was stirred at room temperature for 4 hours. After an aqueous solution of sodium hydrogencarbonate was added for neutralization, extraction with ethyl acetate was conducted. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over sodium sulfate, followed by filtration with a small amount of silica gel. The filtrate was concentrated under reduced pressure, to give 0.342 g of the title compound as a yellow oily substance.

1. temperaturewas heated
2. temperatureunder reflux for 8 hours
3. concentrationAfter the reaction mixture was concentrated
4. extractionthe residue was extracted with ethyl acetate
5. washThe organic layer was washed with water
6. dry with materiala saturated aqueous solution of sodium chloride and dried over sodium sulfate
7. distillationAfter the solvent was distilled off
8. addition5 ml of acetic acid and 0.5 g of reduced iron were added to the residue
9. additionAfter an aqueous solution of sodium hydrogencarbonate was added for neutralization, extraction with ethyl acetate
10. washThe organic layer was washed with water
11. dry with materiala saturated aqueous solution of sodium chloride and dried over sodium sulfate
12. filtrationfollowed by filtration with a small amount of silica gel
13. concentrationThe filtrate was concentrated under reduced pressure