Application of 64248-64-2, These common heterocyclic compound, 64248-64-2, name is 2,5-Difluorobenzonitrile, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Added in the reaction bottle 20g of the 2,5-dichlorobenzonitrile, 12g dry potassium fluoride, used for dissolving sulfolane 34ml 0.55mol/L. Stir until no solid particles. After mixing, heating to 170 C, in 170 C maintain the temperature of 2 hours. Then continue to heating to 210 C, is kept at this temperature for 4 hours, to stop the reaction, the reaction bottle to add new 18mL0.55mol/L sulfolane, the temperature rising to 120 C inject the ammonia 2 hours, the reaction bottle cooling to 30 C, slowly dropping 24mL0.66moL/L sodium nitrite aqueous solution. After the reaction is complete 10g acrylonitrile, heating to 110 C. To fully dissolve the 15g copper powder and 20 ml/L the hydrobromidum, heating to 150 C, maintain 2 hours, to stop the reaction. Dilution with water extraction with ethyl acetate, to obtain in the dilute 40ml0.98mol/L in aqueous solution of sulfuric acid, heating to 110 C hydrolysis 8 hours, cooling to room temperature after the reaction, by adding 400 ml distilled water, once again extracted with ethyl acetate to obtain 15.28g 2-fluoro-5-bromonicotinic acid, to yield 80.12%.
The synthetic route of 64248-64-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Changzhou University; Dong, YanMin; (5 pag.)CN104387264; (2016); B;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts