反应详情

A mixture of 23 parts of methyl 2-methylalanine hydrochloride, 55 parts of phenyl [4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]carbamate. 12.45 parts of sodium hydrogen carbonate, 10 parts of N,N-dimethyl-4-pyridinamine and 300 parts of 1,4-dioxane was stirred overnight at reflux temperature. Water was added till saturation. After stirring for another hour at reflux temperature, the mixture was cooled to room temperature. The product was filtered off, washed with water and 2,2'-oxybispropane and 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 crystallized from 4-methyl-2-pentanone. The product was filtered off and dried. yielding 45.33 parts (84.4%) of 3-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-5,5-dimethyl-2,4-imidazolidinedione; mp. 255.0° C. (intermediate 19).

1. temperatureat reflux temperature
2. temperatureat reflux temperature
3. filtrationThe product was filtered off
4. washwashed with water and 2,2'-oxybispropane
5. custompurified by column chromatography over silica gel using
6. additiona mixture of trichloromethane and methanol (98:2 by volume) as eluent
7. customThe pure fractions were collected
8. customthe eluent was evaporated
9. customThe residue was crystallized from 4-methyl-2-pentanone
10. filtrationThe product was filtered off
11. customdried