HRID129939

反应详情

EQUATION

反应方程式

HRID 129939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.1 g of p-toluenesulphonic acid are added to 49.9 g (0.32 mol) of ethyl cyclopropylcarbonylacetate in 200 ml of dry toluene and the mixture is saturated with ammonia gas at room temperature with stirring. After allowing to stand overnight, the mixture is boiled under reflux for 8 hours in a water separator, ammonia gas being continuously introduced. The mixture is allowed to cool overnight and is filtered, and the toluene solution is concentrated in vacuo and removed by distillation in a high vacuum up to 65° C. from unreacted starting material. The substance is subsequently found in the residue. Yield: 11.9 g (24% of theory).

WORKUP

后处理

  1. additioncontinuously introduced
  2. temperatureto cool overnight
  3. filtrationis filtered
  4. concentrationthe toluene solution is concentrated in vacuo
  5. customremoved by distillation in a high vacuum up to 65° C.