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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of 22.1 g of 4-phenyl-1(2H)-isoquinolone, 20 g of anhydrous potassium carbonate and 100 ml of dimethylformamide was stirred for 2 hours at 100° C. Then, 11 g of 3-chloropropanol was added to the resulting solution and the mixture was stirred at 110° C. for 5 hours. After completion of the reaction, the solvent was distilled off, and the residue was dissolved in dichloromethane. Water was added to the resulting solution and, after thoroughly stirring, the dichloromethane layer was separated and dried over anhydrous sodium sulfate. The solvent was distilled off, and the resulting residue was recrystallized from a mixture of ethyl acetate and petroleum ether to obtain 23 g of 2-(3-hydroxypropyl)-4-phenyl-1(2H)-isoquinolone having a melting point of 84° C. as colorless prisms.
WORKUP
后处理
- stirringthe mixture was stirred at 110° C. for 5 hours
- customAfter completion of the reaction
- distillationthe solvent was distilled off
- dissolutionthe residue was dissolved in dichloromethane
- additionWater was added to the resulting solution
- stirringafter thoroughly stirring
- customthe dichloromethane layer was separated
- dry with materialdried over anhydrous sodium sulfate
- distillationThe solvent was distilled off
- customthe resulting residue was recrystallized from a mixture of ethyl acetate and petroleum ether