反应详情

温度

60 °C

In 4 ml of ethanol was dissolved 280 mg of 2-chloro-3,4-diethyoxycarbonyl-6-(4-methoxyphenyl)-5nitropyridine, whereto 340 mg(8.9 eq.) of reduced iron was added. After the mixture was heated to 60° C., 1.5 ml of conc. hydrochloric acid was added dropwise and the mixture was refluxed. After heating for 20 minutes, the solvent was distilled off. The residue was neutralized with an aqueous solution of sodium hydrogencarbonate, followed by extraction with ethyl acetate. After the precipitate was filtered off, the obtained organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. Thereafter, the solvent was distilled off.

1. additionwas added
2. temperaturethe mixture was refluxed
3. temperatureAfter heating for 20 minutes
4. distillationthe solvent was distilled off
5. extractionfollowed by extraction with ethyl acetate
6. filtrationAfter the precipitate was filtered off
7. washthe obtained organic layer was washed with water
8. dry with materiala saturated aqueous solution of sodium chloride, and dried
9. distillationThereafter, the solvent was distilled off