反应详情

A mixture of 16 parts of 1-benzoyl-1,4-dihydro-4-[(1-methyl-1H-benzimidazol-2-yl)methyl]pyridine and 160 parts of methanol was hydrogenated at normal pressure and at 50° C. with 5 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (97.5:2.5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The oily residue was crystallized from 14 parts of 1,1'-oxybisethane. The product was filtered off and dried, yielding 7.8 parts (58.5%) of 1-benzoyl-4-[(1-methyl-1H-benzimidazol-2-yl)methyl]pyridine; mp. 159.3° C. (32).

1. filtrationthe catalyst was filtered off
2. customthe filtrate was evaporated
3. customThe residue was purified by column chromatography over silica gel using
4. additiona mixture of trichloromethane and methanol (97.5:2.5 by volume) as eluent
5. customThe pure fractions were collected
6. customthe eluent was evaporated
7. customThe oily residue was crystallized from 14 parts of 1,1'-oxybisethane
8. filtrationThe product was filtered off
9. customdried