反应详情

A mixture of 6 parts of 1-(3-chloropropyl)-1H-benzimidazole, 7.6 parts of 4-(diphenylmethoxy)piperidine hydrochloride, 10.6 parts of sodium carbonate and 200 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 4-methyl-2-pentanone-phase is dried, filtered and evaporated. The oily residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The oily residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 1-{3-[4-(diphenylmethoxy)-1-piperidinyl]propyl}-1H-benzimidazole; mp. 110.2° C.

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