HRID130331
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed overnight
- customThe mixture was evaporated to dryness
- additionEtOAc was added
- washthe mixture was washed with water, brine
- dry with materialdried over MgSO4
- customEvaporation
- customgave a crude solid
- customPurification
- washeluted with 45% ethyl acetate in hexane
- customevaporated