HRID454137

反应详情

EQUATION

反应方程式

HRID 454137 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-6-methoxy-7-(3-piperidinopropoxy)quinazoline (400 mg, 1.19 mmol), (prepared as described for the starting material in Example 67), potassium carbonate (255 mg, 1.84 mmol) and 7-hydroxyquinoline (180 mg, 1.32 mmol) in DMF (10 ml) was stirred at 100° C. for 4 hours and then allowed to cool to ambient temperature. The resulting mixture was treated with 1.0 N aqueous sodium hydroxide solution (30 ml) and allowed to stir for 1 hour. The crude solid was collected by filtration and washed with water. The resulting solid was dissolved in dichloromethane and filtered through phase separating paper. The solvent was removed by evaporation to give a solid residue which was recrystallised from acetonitrile to give 6-methoxy-7-(3-piperidinopropoxy)-4-(quinolin-7-yloxy)quinazoline (0.27 g, 52%).

WORKUP

后处理

  1. custom(prepared
  2. temperatureto cool to ambient temperature
  3. stirringto stir for 1 hour
  4. filtrationThe crude solid was collected by filtration
  5. washwashed with water
  6. dissolutionThe resulting solid was dissolved in dichloromethane
  7. filtrationfiltered through phase
  8. customseparating paper
  9. customThe solvent was removed by evaporation
  10. customto give a solid residue which
  11. customwas recrystallised from acetonitrile