HRID657320
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureunder reflux for 4 h
- customAfter removing DMF under reduced pressure
- dissolutionthe residue was dissolved in CH2Cl2 (200 mL)
- washwashed with water (50 mL×2)
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- customAfter evaporation of the solvent
- customthe residue was recrystallized from toluene and EtOH