HRID1029399

反应详情

EQUATION

反应方程式

HRID 1029399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixed solution of 2.1 g of 1-(2-pyrrolidone-5-carbonyl)piperazine, 2.5 g of anhydrous potassium carbonate and 120 ml of acetonitrile was cooled with ice water and 1.1 g of ethyl chlorocarbonate in 10 ml of acetonitrile was dropped therein with stirring. After dropping, the mixture was stirred overnight at room temperature. The solvent was evaporated from the reaction mixture in vacuo, methylene chloride was added to the residue, and insoluble matter was removed therefrom by filtration. The solvent was evaporated in vacuo from the filtrate to give 2.3 g of oily product. This was crystallized from ethyl acetate and further recrystallized to give 2.1 g of desired product, m.p. 147°-148.5° C.

WORKUP

后处理

  1. additionwas dropped
  2. stirringthe mixture was stirred overnight at room temperature
  3. customThe solvent was evaporated from the reaction mixture in vacuo, methylene chloride
  4. additionwas added to the residue, and insoluble matter
  5. customwas removed
  6. filtrationby filtration
  7. customThe solvent was evaporated in vacuo from the filtrate