反应详情

温度

100 °C

To 300 mg of 3,4-diethoxycarbonyl-6-(4-methoxyphenyl)-5-nitro-2(1H)pyridone were added 0.5 ml of phosphorus oxychloride and two drops of DMF. The mixture was heated at 100° C. for 1 hour. After ice water was added, the mixture was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried. The solvent was distilled off. The residue was purified by silica gel column chromatography (eluent:ethyl acetate/hexane 1:1).

1. extractionfollowed by extraction with ethyl acetate
2. washThe organic layer was washed with water
3. dry with materiala saturated aqueous solution of sodium chloride and dried
4. distillationThe solvent was distilled off
5. customThe residue was purified by silica gel column chromatography (eluent:ethyl acetate/hexane 1:1)