HRID1589199

反应详情

EQUATION

反应方程式

HRID 1589199 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
97.5 °C

PROCEDURE

实验过程

A mixture of ethyl thiophene-2-carboxylate (12.0 g.) and ethylenediamine (15.4 ml.) was heated at 95-100° C. for 48 hours. Excess ethylenediamine was removed under reduced pressure and the residue was dissolved in water (150 ml.). The insoluble material [bis(carboxamide)derivative] was removed by filtration. Evaporation of the filtrate gave a residue which was dissolved in toluene (50 ml.). The mixture was evaporated to give N-(2-aminoethyl)-thiophene-2-carboxamide as an oil (12.0 g.) essentially pure by TLC (Rf 0.90; Si02 : 10% v/v methanol in chloroform as eluant) which was used without purification.

WORKUP

后处理

  1. customExcess ethylenediamine was removed under reduced pressure
  2. dissolutionthe residue was dissolved in water (150 ml.)
  3. customThe insoluble material [bis(carboxamide)derivative] was removed by filtration
  4. customEvaporation of the filtrate
  5. customgave a residue which
  6. customThe mixture was evaporated