Preparation method of trifloxystrobin
A technology of trifloxystrobin and solvent, which is applied in the field of trifloxystrobin preparation, can solve problems such as increasing the difficulty of product separation, affecting the yield of trifloxystrobin, and easy hydrolysis, and achieves the goal of green environmental protection, easy solvent, and avoiding hydrolysis in the preparation process Effect
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[0037] A preparation method of trifloxystrobin, which comprises the steps of:
[0038] (1) reacting the raw material A and the base at the first temperature in the presence of the first solvent;
[0039] (2) reacting the substance obtained in step (1) with the raw material B at a second temperature in the presence of the first solvent to generate trifloxystrobin, wherein the first temperature is higher than the second temperature;
[0040] (3) After the reaction in step (2), the step (2) is washed with water, precipitated and crystallized to obtain trifloxystrobin.
[0041] The first solvent in this application is a solvent that is compatible with the raw material A so that the raw material A can be dissolved in the first solvent, and further, the first solvent is a solvent with a lower boiling point and is easy to recover. Preferably, the first solvent includes but not limited to one or more of toluene, xylene, cyclohexane, and methylcyclohexane.
[0042] The first temperat...
Embodiment 1
[0050] Add 40 g of toluene to a 250ml round bottom flask, add 20 g of raw material A and 6.38 g of sodium methoxide under stirring, react for 1 hour in an oil bath at 110°C, then distill off 10 g of solvent, cool the system to 25°C, and add 27.6 g of raw material B Dissolve it in 10 g of toluene, add it dropwise to the above system, and keep it warm at 25°C for about 4 hours until the reaction of raw material B is complete. Stop the reaction, add 20 g of water to the system, remove toluene after the liquid separation, add 50 g of methanol, drop in 20 g of water under stirring, and after 1 hour, suction filter and dry to obtain 37.2 g of the product (purity is greater than 99%, spectrogram like figure 1 Shown), the yield is 94.5%.
Embodiment 2
[0052] Add 60 g of methylcyclohexane into a 250 ml round bottom flask, add 20 g of raw material A and 6.38 g of sodium methoxide under stirring, and react in an oil bath at 100°C for 1 hour, then evaporate 20 g of solvent, and cool the system to 25°C. 27.6 g of raw material B was dissolved in 20 g of methylcyclohexane, added dropwise to the above system, and kept at 25°C for about 4 hours until the reaction of raw material B was complete. Stop the reaction, add 20 g of water to the system, remove methylcyclohexane after liquid separation, add 50 g of methanol, drop in 20 g of water under stirring, and dry by suction filtration after 1 hour to obtain 36.3 g of the product (purity greater than 99 %), the yield was 92.2%.
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