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Fluopyram and synthesis method thereof

A technology of fluopyram and its synthesis method, which is applied in the field of preparation of fine chemical pesticide fungicides, can solve the problems of high dechlorination impurity content, high process risk, and low overall yield, and achieve improved safety and mild reaction Safe and yield-enhancing effects

Active Publication Date: 2022-02-11
利民化学有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The invention provides a method for synthesizing fluopyram, aiming at improving the disadvantages of the prior art, such as high process risk, low overall yield, high dechlorination impurity content, and cumbersome process sections.

Method used

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preparation example Construction

[0028] The embodiment of the present invention provides a synthetic method of fluopyram, comprising:

[0029] S1, reduction reaction;

[0030] The reduction reaction was carried out by mixing 2-acetonitrile-3-chloro-5-trifluoromethylpyridine, aluminum nickel supported catalyst and borohydride.

[0031] Most of the prior art uses hydrogen hydrogenation reduction, but hydrogenation reduction requires high pressure conditions, and hydrogen is flammable, which is easy to cause safety accidents. However, in the embodiment of the present invention, borohydride and aluminum-nickel supported catalysts are used for the reduction reaction. Not only safety is improved, but at the same time, the reaction conditions of this step are mild, which is more conducive to industrial production, and no dechlorination impurities are produced, which also improves the yield of fluopyram.

[0032] Further, the embodiments of the present invention specifically use borohydride and aluminum-nickel suppo...

Embodiment 1

[0051] This example provides a synthesis method of fluopyram, refer to the following synthesis route for synthesis:

[0052] Specific steps are as follows:

[0053] Get 2-acetonitrile-3-chloro-5-trifluoromethylpyridine (content 98%) 20g, sodium borohydride 8g and aluminum-nickel supported catalyst (nickel content 40%, manufacturer Ou Shengshi (Beijing) Technology Co., Ltd. ) 5g were respectively dissolved in 200ml of dichloroethane, and the three stocks of materials were simultaneously pumped into a microwave reactor for microwave reduction reaction. The flow rate of the inlet pump is 5ml / s, and the time for pumping in the 2-acetonitrile-3-chloro-5-trifluoromethylpyridine solution is the start time of the microwave reduction reaction, the reaction time is 5min, the microwave reaction power is 200W, and the reaction temperature 30°C, stirring speed 400r / min. After the reaction, the reaction liquid flows out from the microwave reactor to the alkalization tank, and liquid cau...

Embodiment 2

[0057] This embodiment provides a synthetic method of fluopyram, the specific steps are as follows:

[0058] Get 20g of 2-acetonitrile-3-chloro-5-trifluoromethylpyridine (content 98%), 8g of sodium borohydride and 8g of aluminum-nickel supported catalyst and dissolve them in 200ml of dichloroethane respectively, and the three stocks of materials are pumped into The microwave reduction reaction was carried out in a microwave reactor. Among them, the flow rate of the inlet pump is 5ml / s, and the time for pumping 2-acetonitrile-3-chloro-5-trifluoromethylpyridine solution is the start time of the microwave reduction reaction. The reaction time is 5min, the microwave reaction power is 200W, and the reaction temperature 30°C, stirring speed 400r / min. After the reaction, the reaction liquid flows out from the microwave reactor to the alkalization tank, and liquid caustic soda is added dropwise to make the pH value of the material 11, and the liquid phase analysis of the sample is ca...

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Abstract

The invention relates to the field of preparation of fine chemical pesticide bactericides, in particular to fluopyram and a synthesis method thereof. The synthesis method of the fluopyram comprises the following steps: mixing 2-acetonitrile-3-chloro-5-trifluoromethylpyridine, an aluminum-nickel supported catalyst and hydroboron, and carrying out a reduction reaction. The method aims to overcome the defects that in the prior art, the process risk is high, the total yield is low, the dechlorination impurity content is high, and the working section is tedious. The synthesis method provided by the embodiment of the invention is mild in reaction condition and free of dechlorination impurities, and the yield of the fluopyram can be improved.

Description

technical field [0001] The invention relates to the field of preparation of fine chemical pesticide fungicides, in particular to fluopyram and a synthesis method thereof. Background technique [0002] Fluopyram (common name: Fluopyram) is a benzamide fungicide developed by Bayer, which can prevent botrytis cinerea, powdery mildew, sclerotinia and candida on a variety of crops. It has the characteristics of high safety, basically non-toxic, wide range of action and good bactericidal effect. Since its launch in 2012, fluopyram has been registered and listed in more than 50 countries and regions including the United States, China and the European Union, and has been widely used in more than 70 crops, with a very broad market. [0003] Its mechanism of action is as follows: Fluopyram is also one of the benzamide compounds, except for the unique mechanism of action of these compounds. It also inhibits robe germination, germ tube growth, mycelium growth and spore growth. In pla...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61Y02P20/584
Inventor 许辉李林虎李新生孙敬权陈新安孙丽梅马建军吴新缘
Owner 利民化学有限责任公司
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