HRID463519
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated at 95°-100° C. for 48 hours
- customExcess ethylenediamine was removed under reduced pressure
- dissolutionthe residue was dissolved in water (150 ml.)
- customThe insoluble material [bis(carboxamide)derivative] was removed by filtration
- customEvaporation of the filtrate
- customgave a residue which
- customThe mixture was evaporated