反应详情

A mixture of 5.6 parts of 2-(2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)ethyl methanesulfonate, 4.9 parts of (4-fluorophenyl) (4-piperidinyl) methanone hydrochloride, 8 parts of sodium carbonate and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 7 hours with water-separator. After cooling, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The oily residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 10% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 4-methyl-2-pentanone, yielding 4.3 parts of 1-{2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl}-1,3-dihydro-2H-benzimidazol-2-one; mp. 163.6° C.

1. temperatureAfter cooling
2. customthe layers are separated
3. customThe organic phase is dried
4. filtrationfiltered
5. customevaporated
6. customThe oily residue is purified by column-chromatography over silica gel using
7. additiona mixture of trichloromethane and 10% of methanol as eluent
8. customThe pure fractions are collected
9. customthe eluent is evaporated
10. customThe residue is crystallized from 4-methyl-2-pentanone