HRID463520

反应详情

EQUATION

反应方程式

HRID 463520 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of ethyl nicotinate (21.9 g.) and ethylenediamine (30 ml.) was heated to 100° C. for 16 hours under an atmosphere of argon. Excess ethylenediamine was removed by distillation in vacuo and the residue was dissolved in water (100 ml.) The insoluble material [bis(carboxamido)derivative] was removed by filtration. Evaporation of the filtrate, addition of toluene (50 ml.) followed by re-evaporation gave crude N-(2-aminoethyl)pyridine-3-carboxamide (26.5 g.) as its oily free base, essentially pure by TLC (SiO2 : 10% MeOH/CHCl3) and which was used without purification.

WORKUP

后处理

  1. customExcess ethylenediamine was removed by distillation in vacuo
  2. dissolutionthe residue was dissolved in water (100 ml.) The insoluble material [bis(carboxamido)derivative]
  3. customwas removed by filtration
  4. customEvaporation of the filtrate, addition of toluene (50 ml.)
  5. customfollowed by re-evaporation