HRID598072
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 5-methoxy-3-methyl-1H-quinazoline-2,4-dione (165 mg, 0.800 mmol) and N,N-diisopropylethylamine (0.307 ml, 1.76 mmol) in phosphorus oxychloride (2.2 ml, 24.0 mmol) was refluxed for 18 h with stirring and concentrated to dryness under vacuum. The residue was diluted with water. The aqueous solution was extracted with dichloromethane. The extract was washed with water, dried over magnesium sulfate and concentrated under vacuum to afford 179 mg (99%) of the title compound. The residue was used for the next reaction without further purification.
WORKUP
后处理
- temperaturewas refluxed for 18 h
- concentrationconcentrated to dryness under vacuum
- additionThe residue was diluted with water
- extractionThe aqueous solution was extracted with dichloromethane
- washThe extract was washed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under vacuum