HRID1413515

反应详情

EQUATION

反应方程式

HRID 1413515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6.95 parts of 1-(5-chloropentyl)-1,3-dihydro-3-(1-methylethenyl)-2H-benzimidazol-2-one, 5.15 parts of 1-(diphenylmethyl)piperazine, 5.30 parts of sodium carbonate, 0.1 parts of potassium iodide and 160 parts of 4-methyl-2-pentanone is stirred and refluxed overnight with water-separator. The reaction mixture is cooled to room temperature, water is added and the layers are separated. The organic phase is dried filtered and evaporated. The residue is stirred and refluxed for 30 minutes with 12 parts of a hydrochloric acid solution in 40 parts of ethanol. The whole is evaporated and the residue is crystallized from ethanol, yielding 1-{5-[4-(diphenylmethyl)-1-piperazinyl]pentyl-1,3-dihydro-2H-benzimidazol-2-one dihydrochloride.hydrate; mp. 215.3° C.

WORKUP

后处理

  1. customthe layers are separated
  2. customThe organic phase is dried
  3. filtrationfiltered
  4. customevaporated
  5. stirringThe residue is stirred
  6. temperaturerefluxed for 30 minutes with 12 parts of a hydrochloric acid solution in 40 parts of ethanol
  7. customThe whole is evaporated
  8. customthe residue is crystallized from ethanol