HRID662022

反应详情

EQUATION

反应方程式

HRID 662022 的结构方程式

PROCEDURE

实验过程

To a solution of 2-bromo-4-(bromomethyl)benzonitrile (18.0 g, 65.5 mmol) in DMF (60 mL), potassium phthalide (18.2 g, 98.2 mmol) was added, and then the mixture was stirred under reflux for 4 h. The reaction was allowed to cool to room temperature. After removing DMF under reduced pressure, the residue was dissolved in CH2Cl2 (200 mL), and washed with water (50 mL×2). The organic layer was dried over anhydrous sodium sulfate. After evaporation of the solvent, the residue was recrystallized from toluene and EtOH to give the product, 2-bromo-4-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)methyl]benzonitrile (13.5 g, 61%).

WORKUP

后处理

  1. temperatureunder reflux for 4 h
  2. customAfter removing DMF under reduced pressure
  3. dissolutionthe residue was dissolved in CH2Cl2 (200 mL)
  4. washwashed with water (50 mL×2)
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. customAfter evaporation of the solvent
  7. customthe residue was recrystallized from toluene and EtOH