HRID37512

反应详情

EQUATION

反应方程式

HRID 37512 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 0.30 g of 3,4-diethoxycarbonyl-2-mercapto-5-nitro-6-phenylpyridine, 0.41 g of reduced iron and 7 ml of ethanol was heated to 60° C., followed by addition of 1.7 ml of conc. hydrochloric acid. The mixture was heated under reflux for 30 minutes. After the reaction mixture was concentrated, the concentrate was extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over magnesium sulfate. The concentrate was subjected to silica gel column chromatography with chloroform as the eluent, to give 0.21 g of the title compound as a yellowish orange viscous oily substance.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 30 minutes
  3. concentrationAfter the reaction mixture was concentrated
  4. extractionthe concentrate was extracted with ethyl acetate
  5. washThe extract was washed with an aqueous solution of sodium chloride
  6. dry with materialdried over magnesium sulfate