HRID463519

反应详情

EQUATION

反应方程式

HRID 463519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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; SiO2 : 10% v/v methanol in chloroform as eluant) which was used without purification.

WORKUP

后处理

  1. temperaturewas heated at 95°-100° C. for 48 hours
  2. customExcess ethylenediamine was removed under reduced pressure
  3. dissolutionthe residue was dissolved in water (150 ml.)
  4. customThe insoluble material [bis(carboxamide)derivative] was removed by filtration
  5. customEvaporation of the filtrate
  6. customgave a residue which
  7. customThe mixture was evaporated