HRID634697

反应详情

EQUATION

反应方程式

HRID 634697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6-methoxy-7-(2-methylthioethoxy)-3,4-dihydroquinazolin-4-one (1.07 g, 4.0 mmol), thionyl chloride (20 ml) and DMF (4 drops) was heated at reflux for 2 hours and then allowed to cool. The excess thionyl chloride was removed by evaporation and the residue was azeotroped with toluene. The solid residue was partitioned between aqueous sodium hydrogen carbonate and methylene chloride, the organic phase was separated and washed with brine. The organic phase was passed through phase separating paper, and the solvent removed by evaporation to give 4-chloro-6-methoxy-7-(2-methylthioethoxy)quinazoline (810 mg, 71%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. temperatureto cool
  4. customThe excess thionyl chloride was removed by evaporation
  5. customthe residue was azeotroped with toluene
  6. customThe solid residue was partitioned between aqueous sodium hydrogen carbonate and methylene chloride
  7. customthe organic phase was separated
  8. washwashed with brine
  9. customseparating paper
  10. customthe solvent removed by evaporation