HRID37476

反应详情

EQUATION

反应方程式

HRID 37476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

To 1.0 g of 3,4-diethoxycarbonyl-6-methyl-5-nitro-2-pyridone was added 1.3 ml (3.2 eq.) of phenylphosphonic dichloride. The mixture was heated at 170° C. for 20 mintues. Water was added to the reaction mixture, 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 purified by silica gel column chromatography (eluent:ethyl acetate) to give an oily product.

WORKUP

后处理

  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 over magnesium sulfate
  4. distillationAfter the solvent was distilled off
  5. customthe residue was purified by silica gel column chromatography (eluent:ethyl acetate)
  6. customto give an oily product