反应详情

To a stirred mixture of 4 parts of N-[1-(4-fluorophenylmethyl)-1H-benzimidazol-2-yl]-[1,4'-bipiperidine]-4-amine, 1 part ofN,N-diethylethanamine and 91 parts of dichloromethane was added dropwise a solution of 1.6 parts of 4-fluorobenzoyl chloride in 39 parts of dichloromethane: slightly exothermic reaction, the temperature rises from 25° C. to 30° C. Upon completion, stirring was continued for one hour at room temperature. The reaction mixture was purified by high performance liquid chromatography using a mixture of trichloromethane, hexane and methanol (45:45:10 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 1.8 parts (34%) of 1'-(4-fluorobenzoyl-N-[1-(4-fluorophenylmethyl)-1H-benzimidazol-2-yl]-[1,4'-bipiperidine]-4-amine; mp. 194.3° C.; (compound 18).

1. customslightly exothermic reaction
2. customrises from 25° C. to 30° C
3. customThe reaction mixture was purified by high performance liquid chromatography
4. additiona mixture of trichloromethane, hexane and methanol (45:45:10 by volume) as eluent
5. customThe pure fractions were collected
6. customthe eluent was evaporated