HRID233421

反应详情

EQUATION

反应方程式

HRID 233421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

14.69 g (0.100 mol) of tris-(2-aminoethyl)-amine, dissolved in 20 ml of methanol, is instilled in 103.3 g (1.20 mol) of methyl acrylate with stirring at 20° C. The batch is stirred under argon atmosphere for 5 days at room temperature and for 2 days at 50° C. Then, it is concentrated by evaporation in a vacuum and excess methyl acrylate is removed by azeotropic distillation with toluene. The residue is taken up in 150 ml of methanol and 30 ml of diethyl ether, absorptively precipitated with 150 ml of hexane and, after separation of the hexane phase, concentrated by evaporation in a vacuum. The product is obtained as yellowish liquid, which is further reacted without purification.

WORKUP

后处理

  1. stirringThe batch is stirred under argon atmosphere for 5 days at room temperature and for 2 days at 50° C
  2. concentrationThen, it is concentrated by evaporation in a vacuum and excess methyl acrylate
  3. customis removed by azeotropic distillation with toluene
  4. custom30 ml of diethyl ether, absorptively precipitated with 150 ml of hexane
  5. customafter separation of the hexane phase
  6. concentrationconcentrated by evaporation in a vacuum
  7. customThe product is obtained as yellowish liquid, which
  8. customis further reacted without purification