HRID373928

反应详情

EQUATION

反应方程式

HRID 373928 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.00 g of methyl (E)-4-(4-aminophenyl)-3-butenoate was dissolved in 120 ml of n-propanol, followed by the addition of 30.28 g of 1,1-bis-(methylthio)-2-nitroethylene. The obtained mixture was heated under reflux for 3 hours and distilled to remove the solvent. The residue was purified by silica gel column chromatography (solvent: dichloromethane). The obtained solid was washed with ethyl ether to obtain 9.65 g of the title compound as a yellow powder (yield: 86%).

WORKUP

后处理

  1. temperatureThe obtained mixture was heated
  2. temperatureunder reflux for 3 hours
  3. distillationdistilled
  4. customto remove the solvent
  5. customThe residue was purified by silica gel column chromatography (solvent: dichloromethane)
  6. washThe obtained solid was washed with ethyl ether