反应详情

To a stirred solution of 4.6 parts of 2-amino-4-[(1H-imidazol-1-yl)phenylmethyl]benzamide in 90 parts of tetrahydrofuran were added 3.52 parts of 1,1'-carbonylbis[1H-imidazole]. The mixture was stirred first overnight at room temperature and then for 48 hours at reflux temperature. The solution was concentrated under reduced pressure and the concentrate was treated with water. The product was extracted with dichloromethane. A white product was precipitated in the dichloromethane layer. This product was filtered off and crystallized from hot acetonitrile. The product was filtered off, washed with acetonitrile and 2,2'-oxybispropane and dried in vacuo at 60°-70° C., yielding 1.77 parts (35.4%) of 7-[(1H-imidazol-1-yl)phenylmethyl]-2,4(1H,3H)-quinazolinedione; mp. 287.2° C. (comp. 29).

1. temperaturefor 48 hours at reflux temperature
2. concentrationThe solution was concentrated under reduced pressure
3. additionthe concentrate was treated with water
4. extractionThe product was extracted with dichloromethane
5. customA white product was precipitated in the dichloromethane layer
6. filtrationThis product was filtered off
7. customcrystallized from hot acetonitrile
8. filtrationThe product was filtered off
9. washwashed with acetonitrile and 2,2'-oxybispropane
10. customdried in vacuo at 60°-70° C.