HRID1974854

反应详情

EQUATION

反应方程式

HRID 1974854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

23.5 g (107 mmol) of trimethylsulphoxonium iodide and 3.3 g of sodium hydride (80% strength in paraffin oil) are initially introduced and 80 ml of absolute dimethyl sulphoxide are added dropwise at 10° C. The mixture is stirred for an hour at room temperature and 15.7 g (100 mmol) of ethyl 3-oxopyrrolidine-1-carboxylate [J. Med. Pharm. Chem. 5, 752 (1962)] in 20 ml of absolute dimethyl sulphoxide are then added dropwise in the course of 15 minutes. The mixture is stirred for one hour at room temperature, poured onto a mixture of ice and saturated sodium chloride solution and extracted using diethyl ether. The ether solutions are washed with sodium chloride solution, dried over Na2SO4, concentrated and distilled.

WORKUP

后处理

  1. stirringThe mixture is stirred for one hour at room temperature
  2. extractionextracted
  3. washThe ether solutions are washed with sodium chloride solution
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. distillationdistilled