反应详情

A mixture of 7.3 parts of 1-(6-chlorohexyl)-1,3-dihydro-3-(1-methylethenyl)-2H-benzimidazol-2-one, 5.15 parts of 1-(diphenylmethyl)piperazine, 5.3 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, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is stirred and refluxed for one hour with 12 parts of a concentrated hydrochloric acid solution and 40 parts of ethanol. The solvent is evaporated and the residue is taken up in water. The free base is liberated in the conventional manner with ammonium hydroxide. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is crystallized from methanol. The product is filtered off and recrystallized from N,N-dimethylformamide, yielding 1-{6-[4-(diphenylmethyl)-1-piperazinyl]hexyl}-1,3-dihydro-2H-benzimidazol-2-one; mp. 189.7° C.

1. temperatureThe reaction mixture is cooled
2. customthe layers are separated
3. customThe organic phase is dried
4. filtrationfiltered
5. customevaporated
6. stirringThe residue is stirred
7. temperaturerefluxed for one hour with 12 parts of a concentrated hydrochloric acid solution and 40 parts of ethanol
8. customThe solvent is evaporated
9. extractionThe product is extracted with trichloromethane
10. customThe extract is dried
11. filtrationfiltered
12. customevaporated
13. customThe residue is crystallized from methanol
14. filtrationThe product is filtered off
15. customrecrystallized from N,N-dimethylformamide