3-trifluoromethyl substituted pyrazole derivative and synthesis method thereof
A technology of pyrazole derivatives and trifluoromethyl, applied in the field of 3-trifluoromethyl substituted pyrazole derivatives and synthesis thereof, can solve problems such as unfavorable amplification synthesis, achieve good industrial application prospects, efficient synthesis methods, The effect of high product yield
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Embodiment 1
[0057] This example provides a 3-trifluoromethyl-substituted pyrazole derivative and a preparation method thereof.
[0058] Its preparation method is as follows: in an air atmosphere, in a 25 ml reaction flask equipped with a reflux condenser, add 1 mmol of benzaldehyde, 1.2 mmol of p-toluenesulfonyl hydrazide, 6 ml of toluene, 3 mmol of 1,8- Diazabicycloundec-7-ene, 2 mmol 2-bromo-3,3,3-trifluoropropene, the reaction system was stirred and reacted at 60°C for 6 hours, the heating and stirring were stopped, and water, ethyl acetate Ester extraction reaction solution, the ethyl acetate layer is subjected to vacuum rotary evaporation, solvent removal, and then separated and purified by column chromatography to obtain the target product, the column chromatography eluent used is petroleum ether and ethyl acetate, and the volume ratio is 10:1; the yield of product was 88%.
Embodiment 2
[0060] This example provides a 3-trifluoromethyl-substituted pyrazole derivative and a preparation method thereof.
[0061] Its preparation method is as follows: in an air atmosphere, in a 25 ml reaction flask equipped with a reflux condenser, add 1 mmol of benzaldehyde, 1.2 mmol of benzenesulfonyl hydrazide, 6 ml of toluene, 3 mmol of 1,8-bis Azabicycloundec-7-ene, 2 mmol 2-bromo-3,3,3-trifluoropropene, the reaction system was stirred and reacted at 60°C for 6 hours, stopped heating and stirring, added water, ethyl acetate The reaction solution was extracted, the ethyl acetate layer was rotary evaporated under reduced pressure, the solvent was removed, and then separated and purified by column chromatography to obtain the target product. The eluent of the column chromatography used was petroleum ether and ethyl acetate, and the volume ratio was 10 : 1; The productive rate of product is 77%.
Embodiment 3
[0063] This example provides a 3-trifluoromethyl-substituted pyrazole derivative and a preparation method thereof.
[0064] Its preparation method is as follows: in an air atmosphere, in a 25 ml reaction flask equipped with a reflux condenser, add 1 mmol of benzaldehyde, 1.2 mmol of p-toluenesulfonyl hydrazide, 6 ml of toluene, 3 mmol of lithium tert-butoxide , 2 mmoles of 2-bromo-3,3,3-trifluoropropene, the reaction system was stirred at 60°C for 1 hour, the heating and stirring were stopped, water was added, the reaction liquid was extracted with ethyl acetate, and the ethyl acetate layer was reduced Press rotary steaming, remove the solvent, and then separate and purify by column chromatography to obtain the target product. The column chromatography eluent used is petroleum ether and ethyl acetate, and the volume ratio is 10:1; the yield of the product is 24%.
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