HRID1074615

反应详情

EQUATION

反应方程式

HRID 1074615 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringthe mixture was stirred at 110° C. for 5 hours
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off
  4. dissolutionthe residue was dissolved in dichloromethane
  5. additionWater was added to the resulting solution
  6. stirringafter thoroughly stirring
  7. customthe dichloromethane layer was separated
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationThe solvent was distilled off
  10. customthe resulting residue was recrystallized from a mixture of ethyl acetate and petroleum ether