反应详情

A mixture of 4 parts of 1-(4-chlorobutyl)-1,3-dihydro-2H-benzimidazol-2-one, 4 parts of (4-fluorophenyl) (4-piperidinyl) methanone hydrochloride, 10 parts of sodium carbonate, 0.2 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. After cooling, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The solid 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 2 parts (30%) of 1-{4-[4-(4-fluorobenzoyl)-1-piperidinyl]butyl} -1,3-dihydro-2H-benzimidazol-2-one; mp. 176.5° C.

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