反应详情

5.34 g (40 mmol) of 2-amino-4,5-dicyanoimidazole was dissolved in 130 ml water plus 30 ml conc. hyrdrochloric acid and diazotized by the slow addition (over 5 min) of a solution of 4.0 g of sodium nitrite in 15 ml of water. The mixture was then stirred and cooled to 0°-10° for 45 minutes. The resulting cold suspension of 2-diazo-4,5-dicyanoimidazole was poured into a stirred solution of 12.4 g of sodium sulfite and 2.2 g of sodium hydroxide in 50 ml of water at 0°. An immediate yellow precipitate formed. The mixture was stirred at 0° for 30 minutes and then the yellow solid was filtered and air dried. This gave 0.85 g of 2,2'-azobis(4,5-imidazoledicarbonitrile). Recrystallization from water gave golden plates. UV(CH3CN): 390 nm, k 90.0; sh 375 nm, k 83.4; 237 nm, k 41.3).

1. temperaturecooled to 0°-10° for 45 minutes
2. customAn immediate yellow precipitate formed
3. stirringThe mixture was stirred at 0° for 30 minutes
4. filtrationthe yellow solid was filtered
5. customair dried
6. customRecrystallization from water
7. customgave golden plates