HRID894093

反应详情

EQUATION

反应方程式

HRID 894093 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.4 g of 4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfinic acid (crude product, prepared by reduction of the sulfochloride with sodium sulfite) and 1.4 g of N-hydroxy-N'-butyl-urea are suspended in 40 ml of dioxane and a solution of 1 ml of thionyl chloride in 10 ml of dioxane is added dropwise while stirring. The mixture is then heated for 2 hours to 60° C., whereby a limpid solution is formed. The solution is poured into water, the precipitated substance is treated with dilute ammonia, filtered, acidified and the reaction product is recrystallized from dilute acetone. The N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-butyl-urea obtained melts at 188°-190° C.

WORKUP

后处理

  1. temperatureThe mixture is then heated for 2 hours to 60° C., whereby a limpid solution
  2. customis formed
  3. filtrationfiltered
  4. customthe reaction product is recrystallized from dilute acetone