HRID347444

反应详情

EQUATION

反应方程式

HRID 347444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-cyano-4-hydroxy-7-(3-morpholin-4-ylpropoxy)-5-(tetrahydro-2H-pyran-4-yloxy)quinoline (500 mg) and phosphoryl chloride (2.5 ml) in acetonitrile (1.5 ml) was refluxed and stirred for 4 hours. After cooling, the solution was evaporated to dryness. The flask containing the residue was filled with ice chips and excess concentrated aqueous ammonia (25 ml) was added. This mixture was allowed to warm up while stirring overnight. The product was filtered off and air-dried. The title compound was obtained as a white solid (480 mg, 92%); Mass spectrum: M+H+ 432.

WORKUP

后处理

  1. temperaturewas refluxed
  2. temperatureAfter cooling
  3. customthe solution was evaporated to dryness
  4. additionThe flask containing the residue
  5. additionwas filled with ice chips and excess concentrated aqueous ammonia (25 ml)
  6. additionwas added
  7. temperatureto warm up
  8. stirringwhile stirring overnight
  9. filtrationThe product was filtered off
  10. customair-dried