HRID1987169
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
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
- additionis added in 4 g portions to the refluxing solution
- additionAfter completion of the addition the mixture
- temperatureis heated for 18 h at 105° C
- customThe mixture is then evaporated to dryness
- filtrationThe insoluble material is filtered off
- customthe remaining solution is evaporated to dryness
- customThe crude product is used for the next step without further purification