89534-40-7Relevant articles and documents
Synthesis method of clethodim impurity
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Paragraph 0048-0050; 0055-0058, (2021/06/21)
The present invention provides a synthesis method of a clethodim impurity. The method comprises: dissolving methyl crotonate in DMF, sequentially adding ethanethiol and potassium carbonate, heating, and carrying out a reaction during the stirring process to obtain an ethylthio methyl ester compound; reacting the ethyl thio methyl ester compound with lithium hydroxide monohydrate to obtain ethyl thio acid; carrying out a reaction on ethyl thioacid and dichloromethane to obtain ethyl thioacyl chloride; slowly dropwise adding ethyl sulfenyl acyl chloride into a reaction solution of n-butyllithium, THF and a triketone compound to react to obtain diketone; and oxidizing diketone by hydrogen peroxide, and enabling diketone to react with chloramine to generate the clethodim impurity. The synthesis method of the clethodim impurity provided by the invention can conveniently obtain a large amount of clethodim impurity, avoids huge workload of extracting the impurity from a production sample, plays a role in promoting preparation of an impurity standard substance and quality control of a clethodim product, and can be popularized on a large scale.
