HRID130331

反应详情

EQUATION

反应方程式

HRID 130331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 5,7-dimethoxy-3-(4-methoxyphenyl)-quinazoline-4-one (240 mg, 0.76 mmol), as prepared in Example 18 or 19, and Lawesson's reagent (310 mg, 0.76 mmol) in toluene (4 mL) was refluxed overnight. The mixture was evaporated to dryness. EtOAc was added and the mixture was washed with water, brine and dried over MgSO4. Evaporation gave a crude solid. Purification was performed by flash chromatography on silica gel, loaded with dichloromethane and eluted with 45% ethyl acetate in hexane. The pure fraction was combined and evaporated to give a yellow foam (180 mg, 72%).

WORKUP

后处理

  1. temperaturewas refluxed overnight
  2. customThe mixture was evaporated to dryness
  3. additionEtOAc was added
  4. washthe mixture was washed with water, brine
  5. dry with materialdried over MgSO4
  6. customEvaporation
  7. customgave a crude solid
  8. customPurification
  9. washeluted with 45% ethyl acetate in hexane
  10. customevaporated