反应详情

A mixture of 1.27 parts of 2ethenylpyrazine, 6.48 parts of 1-[(4 fluorophenyl)methyl]-N-(4-piperidinyl)-1H-benzimidazol-2-amine, 0.3 parts of acetic acid and 40 parts of methanol was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (88:12 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was washed with 2,2'-oxybispropane and crystallized from 27 parts of methylbenzene, yielding 2.4 parts of 1-)4-fluorophenylmethyl)-N-[1-[2-(2-pyrazinyl)ethyl]-4-piperidinyl]-1H-benzimidazol-2-amine; mp. 165.3° C. (compound 101).

1. temperaturerefluxed for 48 hours
2. customThe solvent was evaporated
3. customThe residue was purified by column-chromatography over silica gel using
4. additiona mixture of trichloromethane and methanol (88:12 by volume) as eluent
5. customThe pure fractions were collected
6. customthe eluent was evaporated
7. washThe residue was washed with 2,2'-oxybispropane
8. customcrystallized from 27 parts of methylbenzene