139297-65-7Relevant articles and documents
Synthesis method and application of prothioconazole
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, (2020/12/14)
The invention relates to the technical field of chemical drug synthesis, and especially relates to a synthesis method and application of prothioconazole. The synthesis method of prothioconazole comprises the following steps: 1, carrying out an epoxidation reaction on a compound represented by formula IV to obtain a compound represented by formula III; 2, performing nucleophilic addition reaction on the compound of the formula III and triazole to obtain a compound represented by formula II; and 3, carrying out a vulcanization reaction on the compound of the formula II to obtain prothioconazolerepresented by formula I. The prothioconazole is prepared by taking the compound of the formula IV as an initial raw material through the epoxidation reaction, the nucleophilic addition reaction and the vulcanization reaction, so the cost is low, safety and high efficiency are achieved, potential safety hazards are avoided, the overall yield is high, reaction conditions are mild, the raw materialutilization rate is increased, three wastes can be obviously reduced, and the method has certain significance for industrial production.
Preparing method for 2-(2-chlorine benzyl)-2-(1-chloromethyl) ethylene oxide
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, (2019/04/30)
The invention provides a preparing method for 2-(2-chlorine benzyl)-2-(1-chloromethyl) ethylene oxide. The preparing method includes the steps that chlorobenzonitrile II and cyclopropyl formic ether III are subjected to a nucleophilic addition reaction, and an alpha and beta-nitrile ketone compound IV is obtained; the alpha and beta-nitrile ketone compound IV is hydrolyzed and subjected to decarboxylation in acid, and a compound 2-(2-chlorphenyl)-1-cyclopropyl-ethanone V is obtained; the 2-(2-chlorphenyl)-1-cyclopropyl-ethanone V and a chlorinated reagent are subjected to chlorination, and 2-chlorine benzyl-(1-chlorine cyclopropyl) ketone VI is obtained; the 2-chlorine benzyl-(1-chlorine cyclopropyl) ketone VI and sulfur ylide react, and the 2-(2-chlorine benzyl)-2-(1-chloromethyl) ethylene oxide is obtained. According to the preparing method for the 2-(2-chlorine benzyl)-2-(1-chloromethyl) ethylene oxide, through nucleophilic addition, acidic hydrolysis decarboxylation and chloro andcarbonyl epoxidation, a midbody is prepared, a path is simple, the cost of reactant is low, the condition of a four-step reaction is mild, and the 2-(2-chlorine benzyl)-2-(1-chloromethyl) ethylene oxide is better suitable for industrial production.
Preparation method of 2-chlorobenzyl-(1-chloro cyclopropyl) ketone
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Paragraph 0011, (2017/08/30)
The invention relates to a preparation method of 2-chlorobenzyl-(1-chloro cyclopropyl) ketone. The preparation method has the advantages that the reaction condition is mild, the technology is simple and convenient, and the operation is continuous. The preparation method comprises the following steps of under the condition of existence of strong alkaline and a solvent A, using 2-chlorobenzonitrile and 1-chloro cyclopropyl formatepanecarboxylate as raw materials, reacting at the temperature of 50 to 150 DEG C, warming for 1 to 8h, and reacting, so as to obtain an intermediate salt; cooling to 0 to 40 DEG C, adding a solvent B, acidifying the intermediate salt by acid to the pH (potential of hydrogen) value of 1 to 6, stirring for 0.5 to 2h, and separating out an organic phase, so as to obtain an alpha-beta-ketonitrile compound solution; adding inorganic acid into the alpha-beta-ketonitrile compound solution, wherein the molar ratio of alpha-beta-ketonitrile compound to H is 1:(5 to 15), reacting for 18 to 24h, washing the organic phase by water, and distilling to remove the solvent, so as to prepare a sterilizer, namely prothioconazole intermediate 2-chlorobenzyl-(1-chloro cyclopropyl) ketone, wherein the solvent A is methyl alcohol or ethyl alcohol, isopropyl alcohol and the like; the solvent B is water or methyl alcohol, ethyl alcohol, isopropyl alcohol and the like; the acidifying intermediate salt is hydrochloric acid or sulfuric acid, acetic acid and the like.