HRID1729828

反应详情

EQUATION

反应方程式

HRID 1729828 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 5,3 parts of 5-chloro-1,3-dihydro-3-methyl-1-(4-piperidinyl)-2H-benzimidazol-2-one, 6.4 parts of sodium carbonate, 0.2 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 30 minutes with water-separator. After cooling, there are added 7 parts of 1-chloro-4,4-bis(4-fluorophenyl)-butane and stirring at reflux temperature is continued overnight. The reaction mixture is cooled, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The oily residue is triturated in 2,2'-oxybispropane. The product is filtered off, dried and crystallized from 2-propanol, yielding 5-chloro-1-{1-[4,4-bis(4-fluorophenyl)butyl]-4-piperidinyl}-1,3-dihydro-3 -methyl-2H-benzimidazol-2-one; mp. 155.8° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. stirringstirring
  3. temperatureat reflux temperature
  4. temperatureThe reaction mixture is cooled
  5. customthe layers are separated
  6. customThe organic phase is dried
  7. filtrationfiltered
  8. customevaporated
  9. customThe oily residue is triturated in 2,2'-oxybispropane
  10. filtrationThe product is filtered off
  11. customdried
  12. customcrystallized from 2-propanol