反应详情

温度

70 °C

A mixture of 3.6 parts of 1-[5,5-bis(4-fluorophenyl)pentyl]-3-methylpiperazine, 3 parts of N-(4-acetyl-2,6-dichlorophenyl)-2-chloroacetamide, 1.9 parts of N,N-diethylethanamine and 45 parts of N,N-dimethyformamide was stirred for 20 hours at 70° C. The reaction mixture was evaporated and the residue was taken up in a mixture of sodium carbonate and water. The product was extracted with dichloromethane. The extract 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 (98:2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was converted into the hydrochloride salt in 2-propanol and 2,2'-oxybispropane. The product was filtered off and dried in vacuo at 40° C., yielding 1.74 parts (22.8%) of N-(4-acetyl-2,6-dichlorophenyl)-4-[5,5-bis(4-fluoro-phenyl)pentyl]-2-methyl-1-piperazineacetamide dihydrochloride, 2-propanol(1:1), sesquihydrate; mp. 176.3° C. (compound 54).

1. customThe reaction mixture was evaporated
2. additionthe residue was taken up in a mixture of sodium carbonate and water
3. extractionThe product was extracted with dichloromethane
4. washThe extract 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 (98:2 by volume) as eluent
10. customThe pure fractions were collected
11. customthe eluent was evaporated
12. filtrationThe product was filtered off
13. customdried in vacuo at 40° C.