HRID1987169

反应详情

EQUATION

反应方程式

HRID 1987169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

Fumaric acid diethylester (21.6 g; 0.126 mol) is dissolved in toluene (900 ml) and heated at 105° C. A mixture of N-benzylglycine (25 g; 0.151 mol) and paraformaldehyde (25.36 g; 0.844 mol) is added in 4 g portions to the refluxing solution. After completion of the addition the mixture is heated for 18 h at 105° C. The mixture is then evaporated to dryness and suspended in n-hexane. The insoluble material is filtered off and the remaining solution is evaporated to dryness. The crude product is used for the next step without further purification. Yield: 32.5 g (70.3%), ESI-MS: m/z=306 [M+H]+

WORKUP

后处理

  1. additionis added in 4 g portions to the refluxing solution
  2. additionAfter completion of the addition the mixture
  3. temperatureis heated for 18 h at 105° C
  4. customThe mixture is then evaporated to dryness
  5. filtrationThe insoluble material is filtered off
  6. customthe remaining solution is evaporated to dryness
  7. customThe crude product is used for the next step without further purification