反应详情

A mixture of 4.2 parts of 1-(3-chloropropyl)-1,3-dihydro-5-(trifluoromethyl)-2H-benzimidazol-2-one, 3.6 parts of (4-fluorophenyl) (4-piperidinyl) methanone hydrochloride, 10 parts of sodium carbonate, 0.1 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and heated till reflux. Refluxing is continued overnight. After cooling to room temperature, the reaction mixture is poured onto water. The organic phase is separated, dried, filtered and evaporated. The 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 a mixture of 4-methyl-2-pentanone and 2,2-oxybispropane, yielding 1.4 -parts (20%) of 1-{3-[4-(4-fluorobenzoyl)-1-piperidinyl]propyl}-1,3-dihydro-5-(trifluoromethyl)-2H-benzimidazol-2-one; mp. 160.2° C.

1. temperatureheated
2. temperaturetill reflux
3. temperatureRefluxing
4. additionthe reaction mixture is poured onto water
5. customThe organic phase is separated
6. customdried
7. filtrationfiltered
8. customevaporated
9. customThe residue is purified by column-chromatography over silica gel using
10. additiona mixture of trichloromethane and 10% of methanol as eluent
11. customThe pure fractions are collected
12. customthe eluent is evaporated
13. customThe residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2-oxybispropane