反应详情

A mixture of 1.5 parts of N-methyl-N'-nitro-N-nitrosoquanidine, 3.7 parts of N-[1-(2-aminoethyl)-4-piperidinyl]-1-(4-fluorophenylmethyl)-1H-benzimidazol-2-amine and 80 parts of ethanol 50% was stirred overnight at room temperature. The reaction mixture was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (96:4 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2-propanol. The product was filtered off and dried overnight at 110° C., yielding 1.5 parts (33%) of N-[2-[4-[[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]amino]-1-piperidinyl]ethyl]-N'-nitroguanidine; mp. 146.7° C. (compound 23).

1. customThe reaction mixture was evaporated
2. customThe residue was purified by column chromatography over silica gel using
3. additiona mixture of trichloromethane and methanol
4. customThe pure fractions were collected
5. customthe eluent was evaporated
6. customThe residue was crystallized from 2-propanol
7. filtrationThe product was filtered off
8. customdried overnight at 110° C.