反应详情

To a suspension of 4′-cyano-p-toluenesulfonanilide (1153 g (4.23 mol) in acetic anhydride (2306 ml), fuming nitric acid (294.3 g (4.53 mol) was added dropwise, keeping the temperature at 50° C. with stirring, over a period of 100 minutes. After completion of the addition, the reaction mixture was stirred at 50° C. for 1.5 hours. Then, 1.75 ml (0.042 mol) of fuming nitric acid was further added and stirring was continued for another one hour at 50° C. To the resulting mixture, after being left to cool to room temperature, water (7000 ml) was then added to make crystals to deposite. After stirring under cooling with ice for one hour, the crystals were filtered and washed with water to give 1305 g (97%) of 4′-cyano-2′-nitro-p-toluenesulfonanilide as yellow crystals.

1. customat 50° C.
2. additionAfter completion of the addition
3. stirringthe reaction mixture was stirred at 50° C. for 1.5 hours
4. stirringstirring
5. waitwas continued for another one hour at 50° C
6. waitTo the resulting mixture, after being left
7. stirringAfter stirring
8. temperatureunder cooling with ice for one hour
9. filtrationthe crystals were filtered
10. washwashed with water