- Synthesis method for improving purity of fluorochloridone
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The invention discloses a synthesis method for improving the purity of fluorochloridone, and belongs to the technical field of pesticide intermediates. The synthesis method comprises the following steps: S1, taking a compound shown as a formula (III) and allyl chloride as raw materials, taking an alkaline solution or a salt solution as a solvent, carrying out catalytic reaction at 20-25 DEG C under the action of a phase transfer catalyst, and treating after the reaction is finished to obtain a compound shown as a formula (II); S2, taking the compound as shown in the formula (II) as a raw material, taking anhydrous 1, 2-dichloroethane as a solvent, and carrying out reflux reaction at 80-100 DEG C for 4-6 hours under the combined catalytic action of cuprous chloride and 2, 2-dipyridyl, so as to prepare a mixture containing fluorochloridone; and S3, purifying the fluorochloridone. During purification, an extraction solvent is adopted, large-polarity by-products can be removed to a great extent, and residues are simply stirred and washed by n-hexane, so that a fluorochloridone raw material medicine with the purity of more than 95% can be obtained.
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Paragraph 0026; 0028-0030; 0038-0039; 0041-0042; 0048...
(2021/07/10)
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