反应详情

A mixture of 4.5 g of 1-(3-chloropropyl)-1H-benzimidazole, 5.1 g of 1-(diphenylmethyl)piperazine, 3.7 g of sodium carbonate, 0.1 g of potassium iodide and 100 ml of 4-methyl-2-pentanone was stirred overnight at reflux temperature. After cooling, there was added water and the reaction mixture was separated. The organic layer was dried, filtered and evaporated. The residue was purified by column chromatography (silica gel; CHCl3 /CH3OH 95:5). The eluent of the desired fraction was evaporated and the residue was crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane. The product was filtered off and dried, yielding 1.5 g (14.5%) of 1-[3-[4-(diphenylmethyl)-1-piperazinyl]propyl]-1H-benzimidazole; mp. 132.3° C.

1. temperatureat reflux temperature
2. temperatureAfter cooling
3. customthe reaction mixture was separated
4. customThe organic layer was dried
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by column chromatography (silica gel; CHCl3 /CH3OH 95:5)
8. customThe eluent of the desired fraction was evaporated
9. customthe residue was crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane
10. filtrationThe product was filtered off
11. customdried