120068-79-3, Name is 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, 120068-79-3, belongs to pyrazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows.
In a reaction vessel equipped with a mechanical stirrer, a thermometer, a dropping device, and a reflux condenser, nitrogen in the reaction vessel was thoroughly replaced with nitrogen, and then 176 g (0.55 mol) 5-amino-3-cyano-1- (2,6-dichloro-4-trifluoromethylphenyl)pyrazole and 800g chloroform solution (the solution was fully dried over anhydrous sodium sulfate, the amount of desiccant is 500% of the theoretical amount required for the formation of complete hydrate from the free water of sodium sulfate and the system, and the desiccant is filtered and filtered) an additional 130 g (0.60 mol) of the dried salt of p-toluenesulfonic acid dimethylamine, the test solution has a water content of 250ppm (system contains about 0.28g, S Jie 15.4mmol7jO, add 1.18g (7.7mmol) of phosphorus oxychloride,Stirring at room temperature 0.5h, the test solution has a water content of less than 50ppm, achieve moisture control standards, the system was cooled to 0 C, 88.5g (0.58mol) of trifluoromethanesulfonyl chloride was added dropwise and evaporated to dryness, and the temperature was raised to the reflux temperature at the end of the dropwise addition. The raw materials of the pyrazole intermediate disappeared after refluxing for 5h and the temperature was lowered to 10 C, add water 200ml, stirred 0.5h, liquid separation, the organic phase was washed with saturated sodium bicarbonate solution, washed with water, the organic phase was separated, the chloroform was distilled off to obtain fipronil crude. The crude product was recrystallized from toluene to give fipronil 198g, purity 98.5%, the total yield of 81%
Statistics shows that 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile is playing an increasingly important role. we look forward to future research findings about 120068-79-3.