HRID463520
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customExcess ethylenediamine was removed by distillation in vacuo
- dissolutionthe residue was dissolved in water (100 ml.) The insoluble material [bis(carboxamido)derivative]
- customwas removed by filtration
- customEvaporation of the filtrate, addition of toluene (50 ml.)
- customfollowed by re-evaporation