反应详情

A mixture of 5.5 parts of 3-(5-chloro-2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)propyl methanesulfonate, 3.6 parts of (4-fluorophenyl) (4-piperidinyl) methanone, 6 parts of sodium carbonate and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. After cooling, the reaction mixtue is filtered and the filtrate is evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 5% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 4-methyl-2-pentanone. The product is filtered off and recrystallized from 4-methyl-2-pentanone, yielding 0.6 parts (10%) of 5-chloro-1-{3-[4-(4-fluorobenzoyl)-1-piperidinyl] propyl} -1,3-dihydro-2H-benzimidazol-2-one; mp. 163.7° C.

1. temperaturerefluxed overnight
2. temperatureAfter cooling
3. filtrationthe reaction mixtue is filtered
4. customthe filtrate is evaporated
5. customThe residue is purified by column-chromatography over silica gel using
6. additiona mixture of trichloromethane and 5% of methanol as eluent
7. customThe pure fractions are collected
8. customthe eluent is evaporated
9. customThe residue is crystallized from 4-methyl-2-pentanone
10. filtrationThe product is filtered off
11. customrecrystallized from 4-methyl-2-pentanone