反应详情

温度

100 °C

In 2.5 ml of phosphorus oxychloride was suspended 130 mg of 3,4-diethoxycarbonyl-2-hydroxy-6-(4-hydroxyphenyl)-5-nitropyridine, whereto 0.4 ml of DMF was added. The mixture was heated at 100° C. for 30 minutes. Then, 0.4 ml of DMF was added and the mixture was heated for further 30 minutes. After the solvent was distilled off, ice-water was added, followed by neutralization with sodium hydrogencarbonate and extraction with ethyl acetate. After 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).

1. additionwas added
2. temperaturethe mixture was heated for further 30 minutes
3. distillationAfter the solvent was distilled off
4. additionice-water was added
5. extractionfollowed by neutralization with sodium hydrogencarbonate and extraction with ethyl acetate
6. washAfter the organic layer was washed with water
7. dry with materiala saturated aqueous solution of sodium chloride and dried
8. distillationthe solvent was distilled off
9. customThe residue was purified by silica gel column chromatography (eluent:ethyl acetate)