反应详情

5.6 g (54.1 millimoles) of cyanoacetyl chloride were added dropwise to 6.0 g (29.8 millimoles) of 2-(p-aminophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one in 150 ml of absolute tetrahydrofuran at room temperature, while stirring. After the addition was complete, stirring was continued for a further 10 minutes at 50° C. The product was filtered off under suction at 10° C., washed first with tetrahydrofuran and then with water and recrystallized from dimethylformamide/water. 3.6 g (44%) of 2-[p-(cyanoacetylamino)-phenyl]-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one hemihydrate were obtained as pale beige crystals. Mp.: 284° C. (decomposition).

1. additionAfter the addition
2. stirringstirring
3. filtrationThe product was filtered off under suction at 10° C.
4. washwashed first with tetrahydrofuran
5. customwith water and recrystallized from dimethylformamide/water