Flonicamid synthesis method

Through the four-step synthesis method, the problems of low yield and insufficient purity in the synthesis process of sulfenib are solved, and efficient and simple production of sulfenamid is achieved, which is suitable for industrial application.

CN107162966AInactive Publication Date: 2017-09-15WUXI JIABAO PESTICIDE & PHARMA
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Patent Information

Application Number
CN201710418549.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2017-06-06
Publication Date
2017-09-15
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing synthesis process of sulfenamid has low yield, complex operation and low product purity, making it difficult to meet the needs of industrial production.

Method used

A four-step synthesis method is adopted: 4-trifluoromethylnicotinic acid is first synthesized, then converted into 4-trifluoromethylnicotinic acid chloride, and then N-(chloromethyl)-N-(cyanomethyl)-4-trisynthetic acid is synthesized. Fluoromethylpyridine-3-carboxamide is finally reacted with aqueous sodium carbonate solution to obtain sulfonicamid. The method includes specific reaction steps and molar ratios to ensure high efficiency and purity.

Benefits of technology

The high yield, easy operation and high product purity of flunicamid are achieved, which is suitable for the requirements of industrial production.

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Abstract

The invention discloses a flonicamid synthesis method, which comprises: synthesizing 4-trifluoromethylnicotinic acid; synthesizing 4-trifluoromethylnicotinyl chloride; synthesizing N-(chloromethyl)-N-(cyanomethyl)-4-trifluoromethylpyridine-3-carboxamide; carrying out heating reflux on the 4-trifluoromethylnicotinyl chloride, methylenaminoacetonitrile and toluene, carrying out pressure reducing toluene removal to obtain a N-(chloromethyl)-N-(cyanomethyl)-4-trifluoromethylpyridine-3-carboxamide crude product, and refining the crude product to obtain N-(hydroxymethyl)-N-(cyanomethyl)-4-trifluoromethylpyridine-3-carboxamide; and synthesizing flonicamid, wherein the N-(hydroxymethyl)-N-(cyanomethyl)-4-trifluoromethylpyridine-3-carboxamide is cooled, a sodium carbonate aqueous solution is added, stirring is performed at a room temperature, and filtration is performed to obtain a solid, ie., flonicamid. According to the present invention, the synthesis method has advantages of high yield, simple operation and high product purity, and is suitable for industrial production.
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