反应详情

A mixture of 5.6 parts of 6-chloro-1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one, 4.9 parts of (4-fluorophenyl) (4-piperidinyl) methanone hydrochloride, 8.5 parts of sodium carbonate, 0.2 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed overnight with water-separator. After cooling, water is added and the layers are separated. The 4-methyl-2-pentanone-phase is dried, filtered and 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 2-propanol, yielding 1.9 parts (23%) of 6-chloro- 1-{3-[4-(4-fluorobenzoyl)-1-piperidinyl] propyl}-1,3-dihydro-2H-benzimidazol-2-one; mp. 157° C.

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