反应详情

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 slowly combined with ice water. The product is extracted with dichloromethane and purified by chromatography (silica gel, cyclohexane, methylene chloride/acetone 20/1). 1.4 g product are obtained as a solid. M.p=138-141° C.

1. temperatureat reflux temperature
2. stirringThe reaction mixture is stirred for a further 10 minutes
3. temperatureat reflux temperature
4. extractionThe product is extracted with dichloromethane
5. custompurified by chromatography (silica gel, cyclohexane, methylene chloride/acetone 20/1)