HRID1597236

反应详情

EQUATION

反应方程式

HRID 1597236 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7-(3-morpholinopropoxy)-3,4-dihydroquinazolin-4-one (500 mg, 1.7 mmol), thionyl chloride (10 ml) and DMF (0.1 ml) was heated at reflux for 2 hours. The volatiles were removed by evaporation and the residue azeotroped with toluene. The crude product was partitioned between methylene chloride (50 ml) and saturated aqueous sodium hydrogen carbonate solution (50 ml) and the mixture was stirred for 10 minutes. The organic phase was separated and the aqueous phase extracted with methylene chloride. The combined extracts were dried (MgSO4) and the solvent removed by evaporation to give 4-chloro-7-(3-morpholinopropoxy)quinazoline (425 mg, 80%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. customThe volatiles were removed by evaporation
  4. customthe residue azeotroped with toluene
  5. customThe crude product was partitioned between methylene chloride (50 ml) and saturated aqueous sodium hydrogen carbonate solution (50 ml)
  6. customThe organic phase was separated
  7. extractionthe aqueous phase extracted with methylene chloride
  8. dry with materialThe combined extracts were dried (MgSO4)
  9. customthe solvent removed by evaporation