反应详情

A mixture of 24 parts of phenyl[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]carbamate, 15.9 parts of ethyl N-butylglycine, 2 parts of N,N-dimethyl-4-pyridinamine and 200 parts of 1,4-dioxane was stirred and refluxed overnight. Then water was added and stirring was continued for a while. The reaction mixture was cooled, poured onto water and the whole was stirred. The precipitated product was filtered off, washed with water and dissolved in 150 parts of trichloromethane. This solution was stirred for 30 minutes with 3 parts of silica gel. The latter was filtered off and the filtrate was evaporated. The residue was crystallized from butanol. The product was filtered off and dried in vacuo at 60° C., yielding 2.3 parts of 1-butyl-3-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-2,4-imidazolidinedione; mp. 183.7° C. (39).

1. temperaturerefluxed overnight
2. stirringstirring
3. temperatureThe reaction mixture was cooled
4. additionpoured onto water
5. stirringthe whole was stirred
6. filtrationThe precipitated product was filtered off
7. washwashed with water
8. dissolutiondissolved in 150 parts of trichloromethane
9. stirringThis solution was stirred for 30 minutes with 3 parts of silica gel
10. filtrationThe latter was filtered off
11. customthe filtrate was evaporated
12. customThe residue was crystallized from butanol
13. filtrationThe product was filtered off
14. customdried in vacuo at 60° C.