反应详情

温度

25 °C

Pentachloronitrobenzene containing 5-10% hexaxchlorobenzene, (3.0 g, 10.1 mmole) was dissolved in dimethylsulphoxide (35 ml). Hydrazine hydrate (1.25 g, 25 mmole) was added dropwise with stirring at 25° C. A slight 4°-5° C. increase in temperature was recorded and the solution became red-brown. After approximately 20 minutes a white solid began to be precipitated. Stirring was continued for one hour after which time TLC (1:1 ethyl acetate: 60°-80° C. petrol) indicated that the reaction was complete. The mixture was poured into stirred water (200 ml) and the solid filtered off and dried at 50° C. overnight. The TLC and IR was identical to an authentic sample of pentachlorophenylhydrazine. Yield=2.27 g, 80%.

1. temperatureA slight 4°-5° C. increase in temperature
2. customto be precipitated
3. stirringStirring
4. waitwas continued for one hour
5. customafter which time TLC (1:1 ethyl acetate: 60°-80° C. petrol)
6. additionThe mixture was poured
7. stirringinto stirred water (200 ml)
8. filtrationthe solid filtered off
9. customdried at 50° C. overnight