HRID236650

反应详情

EQUATION

反应方程式

HRID 236650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 75.6 gm of sodium hydroxide in 100 ml of water was added to a stirred mixture of 101.4 gm of p-nitrobenzamidine hydrochloride, 70 gm of perchloromethyl mercaptan and 760 ml of dichloromethane, while keeping the temperature below -5° C. After additional 2 hours at -5° C., the resulting suspension was filtered, and the organic phase was separated, evaporated to dryness, and the residual solid was recrystallized from 95% ethanol, yielding 45 gm of the title compound, m.p. 143°-145° C.

WORKUP

后处理

  1. customthe temperature below -5° C
  2. filtrationthe resulting suspension was filtered
  3. customthe organic phase was separated
  4. customevaporated to dryness
  5. customthe residual solid was recrystallized from 95% ethanol