A kind of preparation method of trifloxystrobin
A technology of trifloxystrobin and methyl ketoxime, which is applied in the field of chemical synthesis, can solve the problems of production storage, difficulty in use, unsuitability for industrial production, cumbersome post-processing, etc., and achieve shortened production cycle, simplified post-processing operation, and simple operation easy effect
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Embodiment 1
[0033]Add 20.5Kg (0.1Kmol) m-trifluoromethylacetophenone oxime, 13.8Kg (0.1Kmol) potassium hydroxide solution with a mass fraction of 45%, 40Kg toluene and 0.96Kg tetrabutylammonium bromide catalyst in the reactor , After stirring the reaction at 10°C-25°C for 30min, add 35.8Kg (0.1Kmol) (E)-2-(2'-bromomethylphenyl)-2-oxoacetic acid methyl ester-O at the above temperature - The mixture of methyl ketone oxime and 40Kg toluene takes 3 to 4 hours, after dripping and keeping warm until the residue of m-trifluoromethyl acetophenone oxime is less than 1% (detected by gas chromatography), stop the reaction;
[0034] The reaction solution obtained in step (1) is left to stand and layered, the toluene phase is separated, and then the toluene is recovered by distillation under reduced pressure, and an ethanol solution with a mass fraction of 80% is added to the obtained residue for recrystallization, and then filtered and dried to obtain White or off-white solid, namely the target produ...
Embodiment 2
[0036] In the reactor, add 20.5Kg (0.1Kmol) m-trifluoromethyl acetophenone oxime, 11Kg (0.11Kmol) mass fraction as 40% sodium hydroxide solution, 45Kg toluene and 1.15Kg tetrabutylammonium chloride catalyst, After stirring the reaction at 25°C to 30°C for 30min, add 37.6Kg (0.105Kmol) (E)-2-(2'-bromomethylphenyl)-2-oxoacetic acid methyl ester-O - The mixture of methyl ketone oxime and 45Kg toluene takes 3 to 4 hours, after dripping and keeping warm until the residue of m-trifluoromethyl acetophenone oxime is less than 1% (detected by gas chromatography), stop the reaction;
[0037] The reaction solution obtained in step (1) is left to stand and layered, the toluene phase is separated, and then the toluene is recovered by distillation under reduced pressure, and an ethanol solution with a mass fraction of 80% is added to the obtained residue for recrystallization, and then filtered and dried to obtain White or off-white solid, namely the target product trifloxystrobin 33.7Kg (0...
Embodiment 3
[0039] Add 20.5g (0.1mol) m-trifluoromethylacetophenone oxime, 39g (0.14mol) potassium carbonate solution with a mass fraction of 50%, 60g methylene chloride and 0.82g tetrabutylammonium bromide catalyst in the reaction kettle , after stirring and reacting at 30°C to 40°C for 30min, add 39.3g (0.11mol) (E)-2-(2'-bromomethylphenyl)-2-oxoacetic acid methyl ester within the above temperature range The mixture of O-methyl ketone oxime and 60g of dichloromethane takes 1 to 2 hours, after dripping and keeping warm until the residue of m-trifluoromethyl acetophenone oxime is less than 1% (detected by gas chromatography), stop the reaction;
[0040] The reaction solution obtained in step (1) was left to stand for stratification, the organic phase was separated, and then dichloromethane was recovered by distillation under reduced pressure, and an ethanol solution with a mass fraction of 80% was added to the obtained residue for recrystallization, and then filtered, Dry to obtain a whit...
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