反应详情

A mixture of 6.7 parts of 1-(4-chlorobutyl)-1H-benzimidazole, 5.5 parts of 1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one, 5.3 parts of sodium carbonate, 0.1 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. The reaction mixture is cooled, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is purified twice by column-chromatography over silica gel using first a mixture of trichloromethane and methanol (95:5 by volume) and then a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 4-methyl-2-pentanone. The product is filtered off and dried, yielding 1.8 parts of 1-{1-[4-(1H-benzimidazol-1-yl)butyl]-4-piperidinyl}-1,3-dihydro-2H-benzimidazol-2-one; mp. 157.1° C.

1. temperaturerefluxed overnight
2. temperatureThe reaction mixture is cooled
3. customthe layers are separated
4. customThe organic phase is dried
5. filtrationfiltered
6. customevaporated
7. customThe residue is purified twice by column-chromatography over silica gel using first
8. additiona mixture of trichloromethane and methanol (95:5 by volume)
9. additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
10. customThe pure fractions are collected
11. customthe eluent is evaporated
12. customThe residue is crystallized from 4-methyl-2-pentanone
13. filtrationThe product is filtered off
14. customdried