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With potassium fluoride In N,N-dimethyl-formamide at 140 - 160℃;
In the solution prepared in step (3)29.0 g of KF was charged under stirring,And then incubating the mixture at a temperature of 140-160 DEG C until the content of 2,3,4-trichlorobenzonitrile reaches 2percent(5) under normal pressure to do spin-drying solvent DMF,The resulting brown-yellow granular solid was recrystallized by dissolving 200 mL of toluene,Cooling to about 0 overnight,Filtration,And dried to give 33.8 g of 3-chloro-2,4-difluorobenzonitrile as a pale yellow granular solid in an amount of 98.637percent (GC) in a molar yield of 65.0percent Benzene);
Reference:
[1] Patent: CN106278860, 2017, A, . Location in patent: Paragraph 0023; 0028; 0029
Stage #1: 2,3,4-trichloroaniline With hydrogenchloride; sodium nitrite
Stage #2: potassium cyanide With copper(l) cyanide In water at 20℃; for 0.333333h;
With potassium fluoride; In N,N-dimethyl-formamide; at 140 - 160℃;
In the solution prepared in step (3)29.0 g of KF was charged under stirring,And then incubating the mixture at a temperature of 140-160 DEG C until the content of 2,3,4-trichlorobenzonitrile reaches 2%(5) under normal pressure to do spin-drying solvent DMF,The resulting brown-yellow granular solid was recrystallized by dissolving 200 mL of toluene,Cooling to about 0 overnight,Filtration,And dried to give 33.8 g of 3-chloro-2,4-difluorobenzonitrile as a pale yellow granular solid in an amount of 98.637% (GC) in a molar yield of 65.0% Benzene);