120116-88-3Relevant articles and documents
Preparation method of cyazofamid
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Paragraph 0019; 0024; 0025; 0026-0032; 0033-0039, (2019/01/06)
The invention discloses a preparation method of cyazofamid, comprising the following steps: carrying out a reaction on 5-(para-toluene)-1H-imidazole, anhydrous potassium carbonate, ethyl acetate and N,N-dimethylamino sulfonyl chloride at 50-77 DEG C for 6-12 h, cooling to room temperature, washing with water, extracting, drying, evaporating to remove ethyl acetate to obtain an intermediate A crudeproduct, and recrystallizing to obtain an intermediate A; (2) carrying out a reaction on the intermediate A, copper salt, a cyanation reagent, an oxidizing agent and N,N-dimethylformamide at 110-130DEG C for 6-12 h, cooling to room temperature, recovering N,N-dimethylformamide, washing with water, extracting, drying, evaporating to remove ethyl acetate to obtain an intermediate B crude product,and recrystallizing to obtain an intermediate B; and (3) stirring and carrying out a reaction on the intermediate B, N-chlorosuccinimide and acetonitrile at room temperature for 2-6 h, recovering thesolvent acetonitrile after the reaction, neutralizing to neutral level by adding a sodium bicarbonate solution, extracting, drying, evaporating to remove ethyl acetate to obtain a cyazofamid crude product, and recrystallizing to obtain cyazofamid. The preparation method of the invention has high reaction yield and good selectivity.
Synthesis method of cyazofamid
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, (2018/04/01)
The invention discloses a synthesis method of cyazofamid. The synthesis method of cyazofamid comprises the following steps: synthesizing 2,2-halogenated-4'-methyl acetophenone; synthesizing 1-hydroxy-4-(4-methyl phenyl)-2-oxime imidazole-3-oxide; synthesizing 2-cyan-4-chlorine-5-(4'-methyl phenyl)imidazole; adding methanol into 1-hydroxy-4-(4-methyl phenyl)-2-oxime imidazole-3-oxide, performing ice-water bath reaction, adding sulfoxide chloride, performing temperature-rising reaction, adding acetonitrile and N-chlorosuccinimide, and performing reaction; and synthesizing cyazofamid: adding 2-cyan-4-chlorine-5-(4'-methyl phenyl)imidazole, anhydrous potassium carbonate, ethyl acetate and N,N-dimethylsulfamoyl chloride into a reaction kettle, and performing refluxing reaction. The synthesis method of cyazofamid has the advantages of rich raw material source, easily available raw materials, low cost, mild reaction condition, no need of special equipment, high economic property, high total yield and good industrialized prospect.
A 4-chloro-2-cyano-N, N-dimethyl-5 - (4 the [...] -methyl-phenyl) - 1H-imidazole-1-sulfonamide synthesis method
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, (2017/01/02)
The invention discloses a synthesis method of 4-chloro-2-cyano-N,N-dimethyl-5-(4-methylphenyl)-1H-imidazole-1-sulfonamide (cyazofamid). According to the synthesis method, methylacetophenone is taken as a raw material, selenium dioxide is used for oxidation to prepare an intermediate, namely 2-carbonyl-2-p-benzyl aldehyde, then N,N-dimethylformamide and the like are taken as solvents, thionyl chloride is taken as a chlorinating agent and reducing agent for preparing the intermediate, and then intermediate further reacts with N,N-dimethyl sulfonamide chloride to synthesize the cyazofamid. Compared with the prior art, the synthesis method has the advantages that the reaction period is shortened, the post-treatment process is simplified and the synthesis method is suitable for mass industrial production.