HRID37500

反应详情

EQUATION

反应方程式

HRID 37500 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.379 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine, 0.2 g of (1H-1,2,4-triazole, 0.2 ml of pyridine and 15 ml of 1,2-dichloroethane was reacted at 80° C. for 18 hours. After the reaction mixture was concentrated, the concentrate was extracted with ethyl acetate. The extract was washed with water and a saturated aqueous solution of sodium chloride and dried over sodium sulfate. After the solvent was distilled off, the residue was subjected to silica gel column chromatography (eluent:dichloromethane/ethyl acetate 4:1), to give 0.19 g of the title compound as yellow crystals.

WORKUP

后处理

  1. customwas reacted at 80° C. for 18 hours
  2. concentrationAfter the reaction mixture was concentrated
  3. extractionthe concentrate was extracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materiala saturated aqueous solution of sodium chloride and dried over sodium sulfate
  6. distillationAfter the solvent was distilled off