HRID1838555

反应详情

EQUATION

反应方程式

HRID 1838555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of sodium ethanethiolate (120 mg, 1.5 mmol) and 4-(4chloro-2-fluoroanilino)7-(3-chloropropoxy)-6-methoxyquinazoline (227 mg, 0.57 mmol) in DMF (10 ml) was stirred and heated at 70° C. for 3 hours. The reaction mixture was allowed to cool, was diluted with water and extracted with ethyl acetate (3×75 ml). The extracts were combined, washed with water (×2), and then brine, and dried (MgSO4). The solvent was removed by evaporation and the residue was recrystallised from ethyl acetate/hexane to give 4chloro-2-fluoroanilino)-7-(3-(ethylthio)propoxy)6-methoxyquinazoline (86 mg, 40%).

WORKUP

后处理

  1. temperatureto cool
  2. extractionextracted with ethyl acetate (3×75 ml)
  3. washwashed with water (×2)
  4. dry with materialbrine, and dried (MgSO4)
  5. customThe solvent was removed by evaporation
  6. customthe residue was recrystallised from ethyl acetate/hexane