40800-90-6Relevant academic research and scientific papers
Preparation method of 3-hydroxymethylene benzofuran-2(3H)-one and azoxystrobin intermediates
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, (2021/06/23)
The invention relates to the field of bactericides, and discloses a preparation method of 3-hydroxymethylene benzofuran-2(3H)-one and 3-(alpha-methoxy)-methylene benzofuran-2(3H)-one. The structure of the 3-hydroxymethylene benzofuran-2(3H)-one is as shown in a formula (2). The method comprises the following steps carrying out contact reaction on a compound with a structure as shown in a formula (1) and CO to obtain the compound with the structure as shown in the formula (2). The method provided by the invention is clean in process condition, low in reaction raw material cost and easy to industrialize, and can realize the purpose of green generation;.
Method for improving conversion rate of azoxystrobin
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Paragraph 0066-0069, (2021/03/31)
The invention discloses a method for improving the conversion rate of azoxystrobin. The method comprises the following steps: preparing methyl (E)-2-[2-(6-chloropyrimidin-4-yloxy)phenyl]-3-methoxy acrylate; preparing o-hydroxybenzonitrile; mixing methyl (E)-2-[2-(6-chloropyrimidin-4-yloxy)phenyl]-3-methoxy acrylate, o-hydroxybenzonitrile, potassium carbonate and ketene chloride according to a molar ratio of 30: 35: 50: 1.1, and dissolving the obtained mixture in dimethylformamide to obtain a mixed product; and heating the prepared mixed product, keeping the mixed product at a certain temperature, conducting filtering, carrying out reduced-pressure distillation, performing cooling, separating out crystals, carrying out filtering and washing and performing drying to obtain azoxystrobin. On the basis of the prior art, the synthesis of azoxystrobin is improved in the invention, so the yield of azoxystrobin is effectively increased, the conversion rate of the raw materials including methyl(E)-2-[2-(6-chloropyrimidin-4-yloxy)phenyl]-3-methoxy acrylate and o-hydroxybenzonitrile for azoxystrobin in the process of preparing azoxystrobin is effectively improved, and the production benefit of azoxystrobin is improved.
Synthesis method of methoxybenzofuranone
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Paragraph 0028-0033, (2019/05/08)
The invention discloses a synthesis method of methoxybenzofuranone. The synthesis method comprises the following steps: performing a reaction on o-chlorophenylacetic acid, liquid alkali and a catalyst1, acidifying by using concentrated hydrochloric acid, then distilling for dehydration, cyclizing after completion of the dehydration, then washing with alkali, washing with water and concentrating;performing a reaction on trimethyl orthoformate, acetic anhydride and synthesized benzofuranone, deacidifying, dissolving, washing with water and desolvating after completion of the reaction to obtainthe methoxybenzofuranone. According to the synthesis method, the benzofuranone is firstly synthesized from the o-chlorophenylacetic acid and the methoxybenzofuranone is further synthesized from the benzofuranone, the trimethyl orthoformate and the acetic anhydride; during the reaction, the steps, such as acidifying, dehydrating, washing with the alkali, washing with water and distilling, are continuously carried out, so that not only is the originally synthesized benzofuranone purified and the purity of benzofuranone is improved, but also the purity of the methoxybenzofuranone is improved; after being detecting with high performance liquid chromatography, the purity of the methoxybenzofuranone is as high as 98% or above and the yield can reach 90% or above.
[(6 - Substituted - pyrimidine -4 - oxyacetyl) phenyl] -3 - methoxy methyl acrylate (by machine translation)
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Paragraph 0022; 0023, (2018/11/04)
The invention has the activity of inhibiting crop bacteria [(6 - substituted - pyrimidine - 4 - oxyacetyl) phenyl] - 3 - methoxy methyl acrylate, relates to the technical field of biochemistry. It has the following general structure: It is inhibiting the cucumber wilt disease, peanut pinguis bacteria, germ, galenical wheat, maize leaf spot, watermelon anthrax bacteria, donor bacteria and other applications has good activity. (by machine translation)
Preparation method of azoxystrobin
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Paragraph 0027; 0040; 0050; 0051; 0052; 0053; 0064-0066, (2018/04/02)
The invention discloses a preparation method of azoxystrobin. The preparation method of the azoxystrobin particularly comprises the following steps: performing reaction on hydroxyphenylacetic acid serving as a starting material and trimethyl orthoformate to generate 3-(alpha-methoxy)-methylene benzofuran-2-(3 hydrogen)-ketone, performing reaction on 3-(alpha-methoxy)-methylene benzofuran-2-(3 hydrogen)-ketone, sodium methylate and 4,6-dichloropyrimidine to obtain 3-((alpha)-2-(2-(6-chloropyrimidine-4-yl oxy)phenyl)-methyl 3-methoxyacrylate, performing reaction on 3-((alpha)-2-(2-(6-chloropyrimidine-4-oxy)phenyl)-methyl 3-methoxyacrylate, methanesulfonic acid and methylbenzene to obtain (E)-2-(2-(6-chloropyrimidine-4-yl oxy)phenyl)-methyl 3-methoxyacrylate, and finally performing reaction on (E)-2-(2-(6-chloropyrimidine-4-yl oxy)phenyl)-methyl 3-methoxyacrylate, hydroxybenzonitrile, potassium carbonate, ferric oxide and the like to obtain the azoxystrobin. According to the preparation method provided by the invention, the reaction process is easy to control and the yield of the prepared product is high.
A benzofuran -3 - carboxylic acid (by machine translation)
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Paragraph 0015; 0016; 0018; 0020; 0022; 0024, (2018/07/30)
The invention relates to a benzofuran - 3 - carboxylic acid preparation method, the method using the intermediate 1 as raw materials, under alkaline conditions in the open-loop, the closed-loop process for preparing benzofuran - 3 - carboxylic acid. The method is characterized in that the mild reaction conditions, the operation is simple, high yield, is suitable for industrial production. (by machine translation)
Preparation method of methoxy methene compound
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, (2018/10/19)
The invention relates to a preparation method of a methoxy methene compound. The preparation method comprises the following steps that (1) under the existence of alkaline substances, a compound shownas a formula (1) is subjected to hydrolysis reaction; salt of a compound show as a formula (III) is prepared; (2) methylation with a conventional methylation reagent is directly performed without separation to prepare the compound shown as a formula (1); or the prepared salt of the compound show as the formula (III) is subjected to acidification to prepare the compound show as the formula (III); then, under the acid catalysis, the compound and methyl alcohol take substitution reaction to prepare the compound shown as the formula (I). The process is simple and convenient; the raw materials canbe easily obtained; the cost is low; the reaction conversion rate is high; the selectivity is high. The formulas are shown in the description, wherein R1 is hydrogen or Cl-C4 alkyls; R2 is Cl-C4 alkyl; n is 0 or 1.
Synthetic method for azoxystrobin intermediate
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Paragraph 0023; 0024; 0026; 0027, (2017/12/09)
The invention discloses a synthetic method for an azoxystrobin intermediate. The method comprises the following steps: firstly, benzofuranone, trimethyl orthoformate and acetic anhydride are used as raw materials, reactive distillation operation is performed, and thus condensation substances are obtained by a one-pot method with a high yield; and secondly, a one-pot method reaction is performed on the condensation substances and 2,6-dichloropyrimidine in a methanol solution of sodium methylate; and finally, after the reaction is finished, the acidity is regulated, methanol is recycled, alkali washing is performed, a catalyst of p-toluenesulfonic acid is added to the condensed crude products, a reaction is performed, and thus the azoxystrobin intermediate (E)-2-[2-(6-chloropyrimidin-4-yloxy)phenyl]-3-methoxyacrylate is obtained. The method is simple in operation, high in yield, less in by-products, and suitable for industrialized production.
Compounding method for azoxystrobin
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Paragraph 0013, (2017/10/22)
The invention discloses a compounding method for azoxystrobin. The method comprises the following steps: compounding 3-(-methoxy)-methanoisobenzofuran-2(3-hydrogen-)-hydrogen; compounding 3-((alpha)-2-(2-(6-chloropyrimidine-4-oxygen) phenyl)-3-methyl methoxyacrylate; compounding (E)-2-(2-(6-chloropyrimidine-4-oxygen) phenyl)-3-methyl methoxyacrylate; and compounding azoxystrobin. The compounding method for azoxystrobin, provided by the invention, is characterized by simple operation steps, mild reaction conditions, low operation difficulty, low energy consumption, environment-friendly compounding process, less wastewater and waste emission, easiness in treatment, high yield of obtained azoxystrobin, reusable reagent, reduction of reagent consumption, low compounding cost, capability of realizing clean production and being worthy of popularization.
A kind of preparation method of azoxystrobin (by machine translation)
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, (2016/10/09)
The invention discloses a method for preparation of azoxystrobin, the method includes generating steps of azoxystrobin: by benzofuran -2 (3H)-ketone and methyl ester in the presence of catalyst a hydroformylation reaction, generating 3-formoxyl benzofuran -2 (3H)-one, to the latter with dimethyl sulfate oxidizing reaction to produce a 3-(α-methoxy)-methylene benzofuran -2 (3H)-one, with the 4, 6-dichloro pyrimidine and 2-cyano phenol, generating azoxystrobin, wherein: the molar ratio of the reaction materials: benzofuran -2 (3H)-one: catalyst: methyl ester: the = 1.0 dimethyl sulfate [...] 1.0-2.5 the [...] 1.0-10.0 the [...] 0.9-2.5 ;-10-45°C hydroformylation reaction temperature, reaction time 2-24 hours; a reaction temperature for oxidation 0-60°C, reaction time 1-4 hours. The invention has a comparatively simple process, high yield, the characteristics of relatively low cost. (by machine translation)
