- Triazole compound containing dioxolame and preparation method of intermediate of triazole compound
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The invention relates to a preparation method of a dioxolane-containing triazole compound and an intermediate thereof, and the method comprises the following steps: reacting a compound shown as a formula (V) with a compound shown as a formula (IV) in the presence of Lewis acid to prepare a compound shown as a formula (III); reacting the compound shown in the formula (III) with a compound shown in the formula (II) to prepare the compound shown in the formula (I). According to the technical scheme, a triazole group is introduced into 1H-1, 2, 4-triazole-1-acetic acid, generation of an isomer 1, 3, 4-triazole byproduct is avoided, the reaction yield is increased, and the method has the advantages of being simple and convenient in process route, few in reaction step, simple in process, low in production cost, environmentally friendly, green and safe; the post-treatment of the product only needs a simple solvent crystallization process, a nitric acid salifying method and a high-temperature distillation method do not need to be adopted, the requirements on equipment are reduced and the cost is reduced under the condition of improving the yield and content of the product, and the method is suitable for industrial production.
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- Method for synthesizing high-purity difenoconazole
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The invention discloses a method for synthesizing high-purity difenoconazole, which comprises the following steps: 1) carrying out acylation reaction on 3,4'-dichlorodiphenyl ether to obtain an intermediate I; 2) performing cyclization reaction on the intermediate I to obtain an intermediate II; 3) brominating 1,2,4-triazole to prepare a 1,2,-4-triazole bromide; 4) carrying out bromination reaction on the intermediate II and 1,2,4-triazole bromide to obtain an intermediate III and triazole, and carrying out condensation reaction on the intermediate III and 1,2,4-triazole under the action of potassium hydroxide to obtain a difenoconazole crude product; and 5) refining the difenoconazole crude product to obtain a difenoconazole refined product. The method is low in cost, high in quality andhigh in yield, dibromo and hydrolysis byproducts are hardly generated, and the product content and appearance quality of the difenoconazole refined product are improved.
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Paragraph 0006; 0017-0021
(2021/02/10)
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- Method for converting 4 - H difenoconazole isomer into 1 - H-difenoconazole (by machine translation)
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A method for converting 4 - H-difenoconazole isomer into 1 - H-difenoconazole isomer to obtain an alcohol, 2) reaction of the alcohol and hydrobromic acid to obtain a bromide; 3) separating 1 difenoconazole and 4 - H) 1 - H) from the mixture of 4 - H-difenoconazole and 1 - H-difenoconazole isomer; 4) completely converting 4 - H-difenoconazole isomer into 4 - H-phenylene difenoconazole.) isomer is obtained by dissolving 1) difenoconazole and difenoconazole as a mixture in the presence of a base and a transition metal catalyst to obtain a mixture of difenoconazole and difenoconazole -4 4 - H 1 - H. The method not only can effectively reduce the solid waste problem 4 - H difenoconazole isomer, but also can convert the difenoconazole product into 1 - H difenoconazole product, so that the cost is reduced, the product yield is increased, and the economic benefit is improved. (by machine translation)
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- APPLICATION OF TETRAHYDROBENZAZOLE IN PREPARATION OF AGRICULTURAL FUNGICIDE OR FUNGICIDE COMPOSITION AND PREPARATION METHOD THEREOF
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An application of tetrahydrobenzazole in the preparation of an agricultural fungicide or a fungicide composition and a preparation method therefor. A 4-((-(2-chloro-4-(4-chlorophenoxy)phenyl)-4-methyl-1,3-dioxapentan-2-yl)methyl)-4H-1,2,4-triazole(tetrahydrobenzazole) compound has application in agricultural fungicides, having the structural formula shown in formula I is provided. Also, the embodiments transform waste that can usually only be treated as a hazardous organic waste solid, accounting for 35-40% of the production process of an agricultural fungicide difenoconazole, into a useful pesticide, significantly reducing discharge of hazardous organic waste solids, and alleviating environmental protection pressure on manufacturers. The preparation method of the embodiments can also increase the yield of difenoconazole and reduce costs.
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Paragraph 0053-0055
(2020/04/10)
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- Synthetic process of difenoconazole
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The invention discloses a synthetic process of difenoconazole, comprising the steps of synthesizing 2,4-dichloroacetophenone through ionic liquid acylation using m-dichlorobenzene as a raw material; then synthesizing alpha-bromo-2,4-dichloroacetophenone through a green bromination method; subjecting the alpha-bromo-2,4-dichloroacetophenone and 1,2-propanediol to cyclization to generate a ketal compound that is 2-(2,4-dichlorophenyl)-2-bromomethyl-4-methyl-1,3-dioxolane; subjecting the ketal compound and 1,2,4-triazole potassium to condensation to generate 1-[[2-(2,4-dichlorophenyl)-4-methyl-1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole; and finally subjecting the 1-[[2-(2,4-dichlorophenyl)-4-methyl-1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole and parachlorophenol to etherification to obtain the difenoconazole. The process has advantages of easily available raw materials, a high reaction conversion ratio, few byproducts, capability of being friendly to production environment and a low cost.
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- Preparation method of difenoconazole nitrate
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The invention discloses a preparation method of difenoconazole nitrate. The preparation method comprises the following steps: carrying out a microwave reaction on 2-(bromomethyl)-2-(2- chloro-4-(4-chlorophenoxy)phenyl)-4-methyl-1,3-dioxolame and 1H-1,2,4-triazole in the existence of an acid binding agent, a catalyst and a solvent; carrying out distillation to obtain a crude product of difenoconazole, and dissolving the crude product; dissolving the crude product of difenoconazole, and adding nitric acid to form a salt; and carrying out filtration and drying to obtain a finished product of difenoconazole nitrate. The preparation method of difenoconazole nitrate, disclosed by the invention is more mild in reaction condition, short in reaction time, low in solvent dosage, simple in step, green, environment-friendly and suitable for industrial production, and both the yield and content of a final product are relatively high.
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Paragraph 0032-0056
(2019/04/27)
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- Method for reducing 1,3,4-triazole substituent in 1,2,4-triazole alkylation reaction process
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The invention relates to a method for reducing a 1,3,4-triazole substituent in 1,2,4-triazole alkylation reaction process. The method comprises the steps that 1, 2, 4-triazole and an alkylation reagent are subjected to an alkylation reaction in the presence of an alkali and a catalyst, after the reaction is finished, 1, 2, 4-triazole substituent is obtained through aftertreatment, and the catalystis one or a combination of more of polyether, cyclic crown ether, quaternary ammonium salt, quaternary phosphorus salt, quaternary ammonium base and tertiary amine. The method is simple to operate; the method is wide in application range, the content of the 1, 3, 4-triazole substituent in the alkylation reaction process can be reduced, the yield of the 1, 2, 4-triazole substituent is increased, the reaction time is shortened, the reaction temperature is reduced, solvent use is reduced or avoided, the resource utilization rate is increased, three wastes are reduced, the production cost is reduced, and the method meets the requirements of a green and environment-friendly process.
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Paragraph 0035-0038
(2019/12/25)
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- A triazole fungicide synthetic method
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The invention relates to a synthesis method of a triazole bactericide, which comprises the following steps: carrying out condensation reaction on 4-amino-1,2,4-triazole in the presence of an organic solvent to obtain an organic salt, carrying out deamination reaction on the organic salt in the presence of dilute hydrochloric acid and a sodium nitrate water solution, and after the reaction finishes, carrying out after-treatment to obtain the triazole bactericide. The method avoids generation of the byproduct 1,3,4-triazole, and uses the 4-amino-1,2,4-triazole instead of 4-H-1,2,4-triazole to react with the halogenated compound; the deamination reaction is performed to obtain the single 1,2,4-triazole substitute; and the compound is further purified to satisfy the market demand. Compared with the prior art, the method has the advantages of high yield, low cost, fewer three wastes and the like.
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Paragraph 0043-0046; 0051-0054
(2018/06/21)
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- Synergistic Active Compound Combinations Comprising Phenyltriazoles
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The present invention relates to novel active compound combinations comprising, firstly, at least one known compound of the formula (I) in which R1 and R2 have the meanings given in the description. and at least one further known active compound from groups (2) to (27) listed in the description, which combinations are highly suitable for controlling animal pests such as insects and unwanted acarids and also phytopathogenic fungi.
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- Synergistic Fungidical Active Substance Combinations
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The present invention relates to novel active substance combinations which contain spiroxamine, which is known, a known azole and a known carboxamide and which are very suitable for controlling undesired phytopathogenic fungi.
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