反应详情

温度

70 °C

A mixture of 4.05 parts of 2-chloro-N-(2,6-dichlorophenyl)acetamide, 5.6 parts of 1-[4,4-bis(4-fluorophenyl)butyl]-2-piperazinecarboxamide, 2.94 parts of N,N-diethylethanamine and 63 parts of N,N-dimethylformamide was stirred for 5 hours at 70° C. The reaction mixture was poured onto ice-water. The precipitated product was filtered off and dissolved in dichloromethane. The solution was washed with water, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was converted into the hydrochloride salt in 2-propanone and 2-propanol. The salt was filtered off and stirred for 30 minutes in 1,1'-oxybisethane, yielding 4.54 parts of 3-(aminocarbonyl)-4-[4,4-bis(4-fluorophenyl)butyl]-N-(2,6-dichlorophenyl)-1-piperazineacetamide dihydrochloride monohydrate; mp. 182.7° C. (compound 72).

1. additionThe reaction mixture was poured onto ice-water
2. filtrationThe precipitated product was filtered off
3. dissolutiondissolved in dichloromethane
4. washThe solution was washed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by column-chromatography over silica gel using
9. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
10. customThe pure fractions were collected
11. customthe eluent was evaporated
12. filtrationThe salt was filtered off
13. stirringstirred for 30 minutes in 1,1'-oxybisethane