反应详情

温度

45 °C

To a reaction flask was added 400 milliliters of 95 percent ethanol and 24.2 grams (0.10 mole) of tetrachloropicolinonitrile. The mixture was heated to 45°C. with stirring and 3.7 grams (0.11 mole) of 95 percent hydrazine and 10.1 grams (0.10 mole) of triethylamine was added thereto. The mixture was heated under reflux for 1 hour and the reaction mixture thereafter cooled to 40°C. To this mixture was added 400 grams of an ice-water mixture and the solid 3,5,6-trichloro-4-hydrazinopicolinonitrile product which precipitated was recovered by filtration, water washed and dried. The product was recovered in a yield of 20.6 grams (87 percent of theoretical) melting at 178°-181°C.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 1 hour
3. temperaturethe reaction mixture thereafter cooled to 40°C
4. customthe solid 3,5,6-trichloro-4-hydrazinopicolinonitrile product which precipitated
5. filtrationwas recovered by filtration, water
6. washwashed
7. customdried
8. customThe product was recovered in a yield of 20.6 grams (87 percent of theoretical) melting at 178°-181°C.