HRID634748

反应详情

EQUATION

反应方程式

HRID 634748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 6-methoxy-4-phenoxy-7-(2-thiomorpholinoethoxy)quinazoline (2.0 g, 5 mmol) in 2M hydrochloric acid (25 ml) was heated at 90° C. for 1.5 hours. The mixture was allowed to cool and adjusted to pH7 with solid sodium hydrogen carbonate. Methylene chloride was added and the resulting semi-solid product was isolated by decanting and filtering the aqueous mixture. This product was dissolved in acetone and insoluble material was removed by filtration. The solvent was removed by evaporation and the residue azeotroped with toluene to give 6-methoxy-7-(2-thiomorpholinoethoxy)-3,4-dihydroquinazolin-4-one (1.5 g, 92%) as a white solid.

WORKUP

后处理

  1. temperatureto cool
  2. customthe resulting semi-solid product was isolated
  3. customby decanting
  4. filtrationfiltering the aqueous mixture
  5. dissolutionThis product was dissolved in acetone
  6. custominsoluble material was removed by filtration
  7. customThe solvent was removed by evaporation
  8. customthe residue azeotroped with toluene