HRID1031551

反应详情

EQUATION

反应方程式

HRID 1031551 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14 g (0.06 mol) of crude 1-benzyl-4-chloromethyl-pyrrolidin-2-one, prepared as in Example 1a), 10 g of diethylamine and 50 ml of dimethylformamide are stirred or shaken for 2 hours at 150° C. in the autoclave. The mixture is evaporated to dryness in vacuo and the residue is taken up in methylene chloride then washed first with water and finally the title compound is extracted twice with 25 ml of 2N HCl. The aqueous phase is removed, made alkaline with sodium hydroxide solution and the organic base is extracted with methylene chloride. The methylene chloride phase is concentrated by evaporation and the residue is distilled in vacuo.

WORKUP

后处理

  1. stirringshaken for 2 hours at 150° C. in the autoclave
  2. customThe mixture is evaporated to dryness in vacuo
  3. washthen washed first with water
  4. extractionfinally the title compound is extracted twice with 25 ml of 2N HCl
  5. customThe aqueous phase is removed
  6. extractionthe organic base is extracted with methylene chloride
  7. concentrationThe methylene chloride phase is concentrated by evaporation
  8. distillationthe residue is distilled in vacuo