反应详情

温度

50 °C

A mixture of 9 parts of oxirane, 3.24 parts of 1-(4-fluorophenylmethyl)-N-(4-piperidinyl)-1H-benzimidazol-2-amine and 400 parts of methanol was stirred first overnight at room temperature and further for 4 hours at 50° C. 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, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane, yielding 15 parts of 4-[1-(4-fluorophenylmethyl)-1H-benzimidazol-2-ylamino]-1-piperidineethanol; mp. 138.7° C. (intermediate 93).

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 a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane