HRID37468
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
To 1.0 g of 3,4-diethoxycarbonyl-5-nitro-6-phenyl-2-pyridone was added 1.3 ml (3.37 eq.) of phenylphosphonic dichloride, and the mixture was heated at 150° C. for 2.5 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane 1:2), to give an oily product. Yield: 950 mg (90.5%).
WORKUP
后处理
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materiala saturated aqueous solution of sodium chloride, and dried over magnesium sulfate
- distillationThe solvent was distilled off
- customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane 1:2)
- customto give an oily product