HRID501443
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
5 ml of phosphorus oxychloride and 0.338 g of phosphorus pentachloride were added to 0.383 g of 3-benzyl-4-chloro-1,3-dihydroimidazo[4,5-c]pyridin-2-one, and the mixture was heated under reflux for 24 hours. The solvent was concentrated under reduced pressure, and the residue was poured into 50 g of ice/water. The mixture was extracted with 100 ml of ethyl acetate. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography. Thus, 0.13 g of the title compound was obtained from the fraction eluted with ethyl acetate-hexane (2:1).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 24 hours
- concentrationThe solvent was concentrated under reduced pressure
- additionthe residue was poured into 50 g of ice/water
- extractionThe mixture was extracted with 100 ml of ethyl acetate
- dry with materialThe organic layer was dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography