HRID461333

反应详情

EQUATION

反应方程式

HRID 461333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a dry flask equipped with stirrer, thermometer and reflux condenser is placed 25 ml. of ethanol and sodium metal, 0.253 g. (0.011 g. atom) is added in portions. When the sodium is completely reacted, 3.14 g. (0.01 mole) of 2-(4-cyanopiperazin-1-yl)-4-amino-6,7-dimethoxyquinazoline is added and the resulting mixture is refluxed for 5 hours. After cooling to room temperature, glacial acetic acid is added to neutralize the mixture. After evaporation to dryness, 25 ml. of water and 50 ml. of chloroform are added to the residue. The mixture is transferred to a separatory funnel and the chloroform layer washed again with water, dried over anhydrous sodium sulfate then concentrated to dryness to provide the title compound.

WORKUP

后处理

  1. customTo a dry flask equipped with stirrer
  2. temperaturethermometer and reflux condenser
  3. addition(0.011 g. atom) is added in portions
  4. temperaturethe resulting mixture is refluxed for 5 hours
  5. customAfter evaporation to dryness, 25 ml
  6. additionof chloroform are added to the residue
  7. customThe mixture is transferred to a separatory funnel
  8. washthe chloroform layer washed again with water
  9. dry with materialdried over anhydrous sodium sulfate
  10. concentrationthen concentrated to dryness