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
3.06 g of 3,4-dimethoxyaniline was dissolved in 30 ml of pyridine, to the solution was added in small portions 5.28 g of 5-isoquinolinesulfonyl chloride.HCl with stirring under ice cooling, and the mixture was stirred for 30 minutes, and further stirred at a room temperature overnight. After evaporating off the pyridine under a reduced pressure and additing 20 ml of water, the mixture was extracted twice with 50 ml of chloroform/isopropanol (10:1). The extract was dried over magnesium sulfate and evaporated under a reduced pressure to remove the solvent. To the resulting residue was added 20 ml of benzene/chloroform (3:1), and the mixture was slightly warmed and collected to obtain 5.64 g of the title compound as colorless crystals.
WORKUP
后处理
- stirringfurther stirred at a room temperature overnight
- customAfter evaporating off the pyridine under a reduced pressure
- extractionthe mixture was extracted twice with 50 ml of chloroform/isopropanol (10:1)
- dry with materialThe extract was dried over magnesium sulfate
- customevaporated under a reduced pressure
- customto remove the solvent
- additionTo the resulting residue was added 20 ml of benzene/chloroform (3:1)
- temperaturethe mixture was slightly warmed
- customcollected