HRID634652

反应详情

EQUATION

反应方程式

HRID 634652 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

4-Chloro-6,7-dimethoxyquinazoline (200 mg, 0.89 mmol), (prepared as described for the starting material in Example 1), was added to a solution of 3-hydroxybenzenethiol (168 mg, 1.3 mmol) and N,N-diisopropylethylamine (233 μl, 1.3 mmol) in DMF (5 ml). After heating at 40° C. for 10 minutes, the reaction mixture was allowed to cool, diluted with water, acidified to pH3 and the mixture extracted with ethyl acetate. The organic extract was washed with brine, dried (MgSO4) and the solvent removed by evaporation. The residue was recrystallised from a mixture of ethanol and ether to give 6,7-dimethoxy-4-(3-hydroxyphenylthio)quinazoline (259 mg, 93%) as a white solid.

WORKUP

后处理

  1. temperatureto cool
  2. extractionthe mixture extracted with ethyl acetate
  3. extractionThe organic extract
  4. washwas washed with brine
  5. dry with materialdried (MgSO4)
  6. customthe solvent removed by evaporation
  7. customThe residue was recrystallised from a mixture of ethanol and ether