HRID1088833
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
Into a solution of 4.0 g of this product in pyridinemethylene chloride is added 8.39 g of diazabicyclo[5.4.0]undeca-7-ene. Subsequently, under cooling, a methylene chloride solution of 3.36 g of benzenesulfonyl chloride is added dropwise with stirring. After the reaction, water is added, and the organic layer is separated, followed by evaporation of the solvent. The residue is crystallized from an ethanol-n-hexane mixture, purified through silica gel column chromatography, and recrystallized from an ethyl acetate-n-hexane mixture to give 2.98 g of 5-amino-2-benzenesulfonylaminoindan.
WORKUP
后处理
- temperatureSubsequently, under cooling
- additionis added
- customthe organic layer is separated
- customfollowed by evaporation of the solvent
- customThe residue is crystallized from an ethanol-n-hexane mixture
- custompurified through silica gel column chromatography
- customrecrystallized from an ethyl acetate-n-hexane mixture