A kind of difluoromethyl oxime ether derivative and its synthetic method
A technology of difluoromethyl oxime ether and synthesis method, which is applied in oxime preparation, organic chemistry, etc., can solve the problems of blank synthesis technology research, and achieve the effects of wide substrate adaptability, mild reaction conditions, and good industrial application prospects
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Embodiment 1
[0031] A kind of synthetic method of difluoromethyl oxime ether derivative of the present embodiment, concrete synthetic steps are as follows:
[0032] Under nitrogen atmosphere, in a 25 mL reaction flask equipped with a reflux condenser, add 0.4 mmol acetophenone oxime, 0.6 mmol potassium carbonate, 0.6 mmol α-trifluoromethylstyrene, 2 mL N,N -Dimethylformamide, the reaction system was stirred and reacted at 90°C for 12 hours, stopped heating and stirring, cooled to room temperature, added water, extracted the reaction solution with ethyl acetate, and rotary evaporated the ethyl acetate layer under reduced pressure to remove the solvent, Then separated and purified by column chromatography to obtain the target product, the column chromatography eluent used was petroleum ether:ethyl acetate mixed solvent with a volume ratio of 50:1; the yield of the product was 35%.
Embodiment 2
[0034] A kind of synthetic method of difluoromethyl oxime ether derivative of the present embodiment, concrete synthetic steps are as follows:
[0035] Under nitrogen atmosphere, in a 25 ml reaction flask equipped with a reflux condenser, add 0.4 mmol acetophenone oxime, 0.6 mmol tert-butoxide potassium, 0.6 mmol α-trifluoromethylstyrene, 2 ml N , N-dimethylformamide, the reaction system was stirred and reacted at 90°C for 12 hours, stopped heating and stirring, cooled to room temperature, added water, extracted the reaction solution with ethyl acetate, and rotated the ethyl acetate layer under reduced pressure to remove Solvent, separated and purified by column chromatography to obtain the target product, the column chromatography eluent used is a volume ratio of 50:1 petroleum ether: ethyl acetate mixed solvent; the yield of the product is 52%.
Embodiment 3
[0037] A kind of synthetic method of difluoromethyl oxime ether derivative of the present embodiment, concrete synthetic steps are as follows:
[0038] Under nitrogen atmosphere, in a 25 ml reaction flask equipped with a reflux condenser, add 0.4 mmol acetophenone oxime, 0.6 mmol tert-butoxide lithium, 0.6 mmol α-trifluoromethylstyrene, 2 ml N , N-dimethylformamide, the reaction system was stirred and reacted at 90°C for 12 hours, stopped heating and stirring, cooled to room temperature, added water, extracted the reaction solution with ethyl acetate, and rotated the ethyl acetate layer under reduced pressure to remove Solvent, separated and purified by column chromatography to obtain the target product, the column chromatography eluent used is a volume ratio of 50:1 petroleum ether: ethyl acetate mixed solvent; the yield of the product is 52%.
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