HRID2045821
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
3.9 g 5-fluoro-1-methyl-1,3-dihydro-benzimidazol-2-one are suspended in 80 ml phosphorus oxychloride and the reaction mixture is stirred for 2 hours at reflux temperature. 50 ml diethylaniline are added. The reaction mixture is stirred for a further 10 minutes at reflux temperature and ice water is slowly added thereto. The product is extracted with dichloromethane and purified by chromatography (silica gel, cyclohexane, methylene chloride/acetone 20/1). 1.4 g product are obtained in the form of a solid. M.p.=138-141° C.
WORKUP
后处理
- temperatureat reflux temperature
- stirringThe reaction mixture is stirred for a further 10 minutes
- additionis slowly added
- extractionThe product is extracted with dichloromethane
- custompurified by chromatography (silica gel, cyclohexane, methylene chloride/acetone 20/1)