HRID622410

反应详情

EQUATION

反应方程式

HRID 622410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.646 ml of chloroacetonitrile was added to a solution of 23 mg of metallic sodium in 8 ml of absolute methanol, the mixture was stirred for about 60 minutes at room temperature, 1.70 g of (3R)-3-carbamoyloxypyrrolidine hydrochloride were then added, and the mixture was stirred for a further 3 hours. After completion of the reaction, a small amount of insoluble material was filtered off and the solvent was stripped off from the filtrate. Ether was added to the residue, and the precipitated crystals were collected by filtration and washed with ether, giving 2.20 g of 2-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylchloride hydrochloride.

WORKUP

后处理

  1. stirringthe mixture was stirred for a further 3 hours
  2. customAfter completion of the reaction
  3. filtrationa small amount of insoluble material was filtered off
  4. additionEther was added to the residue
  5. filtrationthe precipitated crystals were collected by filtration
  6. washwashed with ether