HRID46861

反应详情

EQUATION

反应方程式

HRID 46861 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 22.6 parts of 6-chloro-1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one and 300 parts of trichloromethane are added dropwise 32 parts of sulfinyl chloride. Upon completion, stirring is continued for 3 hours at reflux. After stirring with activated charcoal, the reaction mixture is filtered hot over hyflo. The filtrate is evaporated and the residue is dissolved in methylbenzene. The solution is washed a few times with water, dried, filtered and evaporated. The oily residue is triturated in 2,2'-oxybispropane. The solid product is filtered off and dried, yielding 19 parts (77.5%) of 6-chloro-1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one; mp. 122° C.

WORKUP

后处理

  1. temperatureat reflux
  2. filtrationthe reaction mixture is filtered hot over hyflo
  3. customThe filtrate is evaporated
  4. dissolutionthe residue is dissolved in methylbenzene
  5. washThe solution is washed a few times with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customThe oily residue is triturated in 2,2'-oxybispropane
  10. filtrationThe solid product is filtered off
  11. customdried