反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture is then heated for 2 hours to 60° C., whereby a limpid solution
- customis formed
- filtrationfiltered
- customthe reaction product is recrystallized from dilute acetone