HRID408102

反应详情

EQUATION

反应方程式

HRID 408102 的结构方程式

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

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