- Preparation method of picoxystrobin
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The invention belongs to the technical field of bactericides, and particularly relates to a preparation method of picoxystrobin. The invention provides a preparation method of picoxystrobin, which comprises the following steps: mixing 2-(6-trifluoromethylpyridine-2-yloxymethyl) methyl phenylacetate, acetic anhydride and trimethyl orthoformate, and carrying out condensation reaction to obtain the picoxystrobin. According to the invention, 2-(6-trifluoromethylpyridine-2-yloxymethyl) methyl phenylacetate, acetic anhydride and trimethyl orthoformate are used as raw materials, and the 2-(6-trifluoromethylpyridine-2-yloxymethyl) methyl phenylacetate and trimethyl orthoformate are subjected to a condensation reaction under the action of acetic anhydride to obtain picoxystrobin; and acetic anhydride can react with a condensation reaction byproduct to reduce the content of the condensation reaction byproduct, promote the condensation reaction and improve the yield of picoxystrobin. The preparation method provided by the invention is simple in process, mild in reaction condition, low in production cost and beneficial to industrial production.
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Paragraph 0037; 0055-0070
(2021/04/21)
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- Novel process for synthesizing cyproconazole intermediate alpha ketone
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The invention relates to a novel process for synthesizing cyproconazole intermediate alpha ketone, which comprises the steps of reacting a metered potassium hydroxide aqueous solution with 2-fluorine-5-trifluoromethylpyridine, neutralizing with sulfuric acid, filtering, washing, drying to obtain trifluoropyridinol, and reacting DMF, trifluoropyridinol, methyl o-chloromethylphenylacetate and sodiumhydroxide to obtain ether ester; then reacting toluene, ether ester, methyl formate and sodium hydroxide for desolvation to obtain enol; and finally reacting dichloromethane, enol, dimethyl sulfate and sodium hydroxide, filtering and drying to obtain a finished picoxystrobin product, so that the whole reaction condition is mild, the operation is simple, the method is a relatively ideal industrialsynthesis route, the total synthesis yield reaches 65% or above, and the product content reaches 97%.
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Paragraph 0021; 0022
(2020/12/15)
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- Method for synthesis -2- of 3- methyl ester compound (methyl ethyl ester) of methyl ethyl ester (methyl) ethyl ester
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The invention relates to a synthesis method of 3-methoxy-2-aryl(methyl)acrylate compounds, which comprises the following steps: by using phenylmethyl acetate with or without substituting groups as a raw material, carrying out formylation reaction at -20-100 DEG C for 4-6 hours in a nitrogen atmosphere in the presence of Lewis acid in an aprotic solvent neutralized formylation reagent, dissociating with an organic base, hydrolyzing with hydrochloric acid, and stratifying, wherein the organic layer is an intermediate; carrying out methylation reaction on the intermediate, benzyltriethylammonium chloride, a methylation reagent and an inorganic base at 20-100 DEG C for 1-3 hours; after the reaction finishes, washing with water, desolventizing, and recrystallizing or distilling while depressurizing to obtain the product. The invention has the advantages of fewer processing steps (the methylation reaction can be directly carried out without purifying and separating the intermediate product), favorable selectivity, higher yield and low cost; and the reaction process is easy to control, and is safe and easy to amplify.
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Paragraph 0030-0045
(2019/12/25)
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- Preparation method of picoxystrobin
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The invention provides a preparation method of picoxystrobin. The preparation method includes the following steps: reacting an alkali metal salt of 2-hydroxy-6-trifluoromethylpyridine with (E)-3-methoxy-2-(2-halomethylphenyl)-2-methyl acrylate in a solvent to obtain the picoxystrobin, wherein the alkali metal salt of the 2-hydroxy-6-trifluoromethylpyridine is prepared by a hydrolysis reaction of 2-halo-6-trifluoromethylpyridine and alkali metal hydroxide. The preparation method provided by the invention saves the use of an acid binding agent in a condensation step and avoids tedious steps suchas acidification and drying in the hydrolysis reaction. After two steps of separation, the total yield is over 82%, and the product content is 97%-98%. A by-product is only a single inorganic salt, which reduces the equipment cost of solvent recovery and saves the use of acid and alkali, thereby reducing the material cost. The preparation method is suitable for industrial production and can generate high economic benefit.
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- Silver-Catalyzed Olefination of Acetals and Ketals with Diazoesters to β-Alkoxyacrylates
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The first silver-catalyzed reaction of acetals or ketals with diazoesters leading to trisubstituted or tetrasubstituted β-alkoxyacrylates is now reported. A broad range of acetals and ketals bearing different substituents is compatible with this protocol and thus provides an attractive approach for the synthesis of complex β-alkoxyacrylates. The power of this method was further demonstrated by the successful synthesis of picoxystrobin, which is one of the most popular agricultural fungicides commercialized by Dupont.
- Li, Jiawen,Qian, Bo,Huang, Hanmin
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supporting information
p. 7090 - 7094
(2018/11/23)
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- Method for preparing alkoxy acrylate
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The invention discloses a method for preparing an alkoxy acrylate. The method comprises that diazo ester and substituted acetal or ketal as raw materials undergo an alkenylation reaction in the presence of Lewis acid as a catalyst at 50-120 DEG C for 1-24h, then the solvent is drained through pumping and the product is subjected to column chromatography separation so that the alkoxy acrylate compound is obtained. The reaction raw materials and the catalyst are easily available and cheap, the synthesis process is simple, the synthesis cost is greatly reduced, the reaction conditions are mild, the yield is high, the industrialization is easy, the reaction raw materials and the catalyst are clean and non-toxic, and the environmental pollution is small.
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Paragraph 0094; 0097
(2018/11/27)
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- NOVEL CRYSTALLINE FORM OF PICOXYSTROBIN, METHOD OF PREPARING AND USE OF THE SAME
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A novel crystalline form of the compound of formula (I) (picoxystrobin) is provided. The novel crystalline form of picoxystrobin may be prepared by crystallization from solution in a suitable solvent. Fungicidal compositions comprising the novel crystalline form, a method for controlling fungal infestations at a locus and a use of the novel crystalline form are also provided.
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- Methoxy acrylic acid esters bactericide preparation method
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The invention relates to a method for preparing strobilurin fungicide. The method comprises the following steps: (1) mixing the compound in formula (II) with the compound in formula (III) for reaction for 5 to 10 h at the temperature of 90 to 120 DEG C to obtain the compound in formula (IV), wherein the compound in formula (III) is acetal of formamides compound, R1, R2 and R3 are substituted alkyl or aryl; and (2) hydrolyzing the compound in formula (IV) under an acidic condition, and then stirring the hydrolyzed product at the room temperature for 2 to 4 h under the condition of alkali, methylating reagent and phase transfer catalyst to obtain the product, wherein X is 6-(2'-cyanophenoxyl) pyrimidine-4-oxy or 6-trifluoromethylpyridine-2-oxymethyl; 6-(2'-cyanophenoxyl) pyrimidine-4-oxy or 6-trifluoromethylpyridine-2-oxymethyl;[2-[[[[4-(4-chlorophenyl)-but-3-en-2-yl]imido]oxy]methyl]phenyl]; and 2-(2-((3-butyl-4-methyl-coumarin-7-yloxy)metyl)phenyl). The total yield of the method reaches above 85%.
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Paragraph 0099; 0100; 0101
(2016/10/09)
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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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- Process for the preparation of 2-(6-substituted pyrid-2-yloxymethyl) phenylacetate
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PCT No. PCT/GB96/01311 Sec. 371 Date Dec. 2, 1997 Sec. 102(e) Date Dec. 2, 1997 PCT Filed Jun. 3, 1996 PCT Pub. No. WO97/01538 PCT Pub. Date Jan. 16, 1997A process for preparing 2-(6-substituted pyrid-2-yloxymethyl)phenyacetates especially useful as intermediates for producing agricultural fungicides. The invention provides a compound having the formula (I): wherein A and D are independently selected from the group comprising halo, hydroxy, halo(C1-4)alkyl, C1-4alkoxy, thio(C1-4)alkoxy, halo(C1-4)alkoxy, phenyl, phenoxy, nitro, amino, aclyamino, cyano, carboxy, C1-4 alkoxycarbonyl and C1-4 alkylcarbonyloxy, or D is C1-4 alkyl, and m is 0 or an integer of from 1 to 3. The process comprises treating a compound of formula (II): wherein A, D and m are defined as above and M is a metal atom, with a compound of formula (III): wherein L is a leaving group.
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