HRID1791523

反应详情

EQUATION

反应方程式

HRID 1791523 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 4-chloro-7-(3-(1,1-dioxothiomorpholino)propoxy)-6-methoxyquinazoline (220 mg, 0.57 mmol), potassium carbonate (106 mg, 0.77 mmol) and 7-hydroxyquinoline (111 mg, 0.76 mmol) in DMF (7.5 ml) was stirred at 100° C. for 5 hours then allowed to cool to ambient temperature. The reaction mixture was treated with 1M aqueous sodium hydroxide solution (40 ml) and stirred at ambient temperature for a few minutes. The crude solid was collected by filtration washing with water. The resultant solid was dissolved in dichloromethane (2 ml) and was filtered through phase separating paper. The filtrate was evaporated under vacuum to give a solid residue which was triturated with ether, filtered and dried to give 7-(3-(1,1-dioxothiomorpholino)propoxy)-6-methoxy-4-(quinolin-7-yloxy)quinazoline (205 mg, 73%).

WORKUP

后处理

  1. temperatureto cool to ambient temperature
  2. stirringstirred at ambient temperature for a few minutes
  3. filtrationThe crude solid was collected by filtration
  4. washwashing with water
  5. dissolutionThe resultant solid was dissolved in dichloromethane (2 ml)
  6. filtrationwas filtered through phase
  7. customseparating paper
  8. customThe filtrate was evaporated under vacuum
  9. customto give a solid residue which
  10. customwas triturated with ether
  11. filtrationfiltered
  12. customdried