反应详情

温度

100 °C

In 6.5 ml of phosphorus oxychloride was dissolved 2.5 g of 3,4-diethoxycarbonyl-5-nitro-6-phenyl-2pyridone, followed by addition of 1 ml of DMF. The mixture was heated at 100° C. for 30 minutes. After the reaction mixture was concentrated under reduced pressure, an aqueous solution of sodium hydrogencarbonate was added to the residue for neutralization, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After the solvent was distilled off, the residue was subjected to silica gel column chromatography (eluent:ethyl acetate/hexane 1:2), to give 1.9 g of the title compound as yellow needles.

1. concentrationAfter the reaction mixture was concentrated under reduced pressure
2. additionan aqueous solution of sodium hydrogencarbonate was added to the residue for neutralization
3. extractionfollowed by extraction with ethyl acetate
4. washThe organic layer was washed with water
5. dry with materiala saturated aqueous solution of sodium chloride and dried over magnesium sulfate
6. distillationAfter the solvent was distilled off