反应详情

A mixture of 5 parts of 1,1'-(5-chloropentylidene)bis(4-fluorobenzene), 5 parts of 3-(aminocarbonyl)-N-(2,6-dichlorophenyl)-1-piperazineacetamide, 2.2 parts of sodium carbonate, 0.1 parts of potassium iodide and 120 parts of 4-methyl-2-pentanone was stirred and refluxed for 24 hours. The reaction mixture was cooled and purified by column-chromatography (2x) over silica gel using first a mixture of trichloromethane and methanol (95:5 by volume) and then a mixture of trichloromethane and methanol (97:3 by volume) as eluents. The pure fractions were collected and the eluent was evaporated. The residue was converted into the hydrochloride salt in acetonitrile and 2-propanol. After stirring for one hour at room temperature, the salt was filtered off and dried, yielding 1.53 parts of 3-(aminocarbonyl)-4-[4,4-bis(4-fluorophenyl)pentyl]-N-(2,6-dichlorophenyl)-1-piperazineacetamide dihydrochloride monohydrate; mp. 206.2° C. (compound 49).

1. temperaturerefluxed for 24 hours
2. temperatureThe reaction mixture was cooled
3. custompurified by column-chromatography (2x) over silica gel using first
4. additiona mixture of trichloromethane and methanol (95:5 by volume)
5. additiona mixture of trichloromethane and methanol (97:3 by volume) as eluents
6. customThe pure fractions were collected
7. customthe eluent was evaporated
8. stirringAfter stirring for one hour at room temperature
9. filtrationthe salt was filtered off
10. customdried