HRID5746

反应详情

EQUATION

反应方程式

HRID 5746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringfurther stirred at a room temperature overnight
  2. customAfter evaporating off the pyridine under a reduced pressure
  3. extractionthe mixture was extracted twice with 50 ml of chloroform/isopropanol (10:1)
  4. dry with materialThe extract was dried over magnesium sulfate
  5. customevaporated under a reduced pressure
  6. customto remove the solvent
  7. additionTo the resulting residue was added 20 ml of benzene/chloroform (3:1)
  8. temperaturethe mixture was slightly warmed
  9. customcollected