Chlorine → 3,4,6-Trichloropyridazine

To a dry three-necked flask equipped with a refluxing condensor and a ventiduct (connected with a safety flask), 3,6-dichloropyridazine (purchased from Nanjingtianzunzezhong Chemical Agents Company) and anhydrous aluminum trichloride were added, heated by using external heat source to 120° C. to melt reactants, Cl2 gas was fed at this temperature for 3 hours, then the reaction was stopped, cooled to room temperature, trichloromethane was added to dissolve the product, the trichloromethane solution was washed with saturated sodium chloride aqueous solution for twice, the water phase was extracted with trichloromethane for twice, all trichloromethane solutions were combined together and dried over anhydrous sodium sulfate, after trichloromethane was removed by evaporation under vacuum, a reduced pressure distillation was employed to collect fraction of 110-114° C./8 mmHg or 128˜9° C./18 mmHg, a white solid was coagulated in a receiving flask. Yield: 55%, m.p. 57˜58° C.

1. customTo a dry three-necked flask equipped with a refluxing condensor
2. temperatureheated
3. customto 120° C.
4. dissolutionto dissolve the product
5. washthe trichloromethane solution was washed with saturated sodium chloride aqueous solution for twice, the water phase
6. extractionwas extracted with trichloromethane for twice, all trichloromethane solutions
7. dry with materialdried over anhydrous sodium sulfate
8. customafter trichloromethane was removed by evaporation under vacuum
9. distillationa reduced pressure distillation
10. customto collect fraction of 110-114° C./8 mmHg or 128˜9° C./18 mmHg
11. customa white solid was coagulated in a receiving flask

ORD record

ord-d5807c38b2fc448281e8828b3344dac1

Source dataset

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08410105B2