反应详情

温度

100 °C

A mixture of 21.3 parts of 3-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-5,5-dimethyl-2,4-imidazolidinedione, 7.5 parts of 3-chloro-2-butanone, 6.0 parts of potassium carbonate and 180 parts of N,N-dimethylformamide was stirred overnight at 100° C. After cooling, the reaction mixture was diluted with 700 parts of water. The crystallized product was filtered off and purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (98.5:1.5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. After trituration of the residue in methanol, the product was filtered off and crystallized from 4-methyl-2-pentanone, yielding 7.77 parts (30.9%) of 3-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-5,5-dimethyl-1-(1-methyl-2-oxopropyl)-2,4-imidazolidinedione; mp. 225.9° C. (intermediate 20).

1. temperatureAfter cooling
2. filtrationThe crystallized product was filtered off
3. custompurified by column chromatography over silica gel using
4. additiona mixture of trichloromethane and methanol (98.5:1.5 by volume) as eluent
5. customThe pure fractions were collected
6. customthe eluent was evaporated
7. filtrationAfter trituration of the residue in methanol, the product was filtered off
8. customcrystallized from 4-methyl-2-pentanone