220368-29-6Relevant articles and documents
A multiplex lateral flow immunochromatography assay for the quantitative detection of pyraclostrobin, myclobutanil, and kresoxim-methyl residues in wheat
Lin, Lu,Xu, Xinxin,Song, Shanshan,Xu, Liguang,Wu, Xiaoling,Liu, Liqiang,Kuang, Hua,Xu, Chuanlai
, (2022/01/11)
We produced three monoclonal antibodies with high specificity and sensitivity, and developed a lateral flow immunochromatography assay (LFIA) for the qualitative and quantitative detection of pyraclostrobin (PYR), myclobutanil (MYC), and kresoxim-methyl (KRE) in wheat. In the qualitative analysis, the cut-off values of LFIA were 400, 200, and 800 ng/g for PYR, MYC, and KRE in wheat, respectively. Based on the results obtained from the membrane strip reader, we generated calibration curves for the quantitative analysis. PYR, MYC, and KRE monoclonal antibodies (mAbs) had half maximal inhibitory concentrations (IC50) of 25.4, 17.7, and 94.6 ng/g, respectively, and limit of detection (LOD) of 2.5, 2.0, and 8.8 ng/g, respectively. The linear detection scopes were 5.6–116.5, 4.2–74.4, 23.4–383.3 ng/g for PYR, MYC, and KRE, respectively. The intra-assay recoveries ranged from 89.2% to 101.7%, and the coefficients of variation ranged from 4.6% to 6.5%. The inter-assay recoveries ranged from 88.7% to 102.7%, with the coefficients of variation ranged from 7.2% to 9.1%. Thus, our developed LFIA is suitable for the qualitative and quantitative detection of PYR, MYC, and KRE residues in wheat.
Synthesis of 2 [(N-4-chlorphenyl)-1H-pyrazol-3-yloxymethyl] nitrobenzene
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Paragraph 0028-0029; 0032-0035; 0038-0041; 0044-0047; ..., (2021/11/10)
The invention discloses synthesis of 2 [(N-4-chlorphenyl)-1H-pyrazole-3-yloxymethyl] nitrobenzene, which comprises the following steps of: synthesizing o-nitrobenzyl iodide from o-nitrotoluene, potassium iodide and hydrogen peroxide in a diluted hydrochloric acid system, and then reacting the o-nitrobenzyl iodide with 1-(4-chlorphenyl)-3-pyrazole alcohol to obtain 2 [(N-4-chlorphenyl)-1H-pyrazole-3-yloxymethyl] nitrobenzene. According to the synthetic method of the 2 [(N-4-chlorphenyl)-1H-pyrazol-3-yloxymethyl] nitrobenzene, almost no by-product is generated, diiodo compounds are not easy to generate, and the conversion rate of o-nitrotoluene is high and can reach 99% or above.
Apparatus and method for producing 2 - [(N - P-chlorophenyl) -3 -pyrazyloxymethyl] nitrobenzene (by machine translation)
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Paragraph 0030-0048, (2020/08/06)
The invention discloses a production device and method for 2 - [(N -P-chlorophenyl) -3 - pyrazyloxymethyl] nitrobenzene, which comprises a batching kettle A, a storage tank A, a storage tank B, a compounding kettle B, a crystallization kettle, a tubular reactor first reaction zone, a tubular reactor second reaction zone and a tubular reactor third reaction zone. To the invention, continuous production is realized; 2 - [(N-4 - Chlorophenyl) -3 - pyrazyloxymethyl] nitrobenzene is synthesized by a tubular reactor, and the problems of low content and yield, serious environmental pollution, large wastewater amount and complicated steps and low automation degree are solved in the background art. (by machine translation)
Substituted amide compound and preparation method and application thereof
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Paragraph 0141-0144; 0167-0170, (2020/03/05)
The invention belongs to the technical field of bactericides, and particularly relates to an amide compound represented by a formula (I) in the specification or a pharmaceutically acceptable salt thereof. The compound of the formula (I) shows good activit
Preparation method for high-purity pyraclostrobin
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, (2019/04/02)
The invention relates to the technical field of compound synthesis, in particular to a preparation method for high-purity pyraclostrobin. The pyraclostrobin is synthesized from p-chloroaniline and o-nitrosotoluene as initial raw materials through the steps of diazotizing, cyclizing, oxidizing, bromizing, condensating, reducing, acylating, methylating and the like. According to the preparation method, the problem that the purity of the pyraclostrobin in the prior art is low is solved; and the preparation method for the pyraclostrobin has the advantages of high yield, high purity and high material utilization rate.
Preparation method of high-purity pyraclostrobin
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Paragraph 0037; 0038; 0044; 0045; 0051; 0052, (2018/06/15)
The invention provides a preparation method of high-purity pyraclostrobin. The high-purity pyraclostrobin is prepared by taking 1-(4-chlorophenyl)-3-hydroxy-1-h-pyrazole and O-nitrobenzyl bromide as raw materials and through condensation, reduction, esterification, methylation and mixed solvent separation and purification. By adopting the preparation method provided by the invention to prepare thehigh-purity pyraclostrobin, the preparation method has the characteristics that the cost is low, the product purity is high, the product yield is high, the raw materials are easy to obtain, and the like; the recycling and reusing rate of a solvent required for reaction is high, the three wastes can be preferably treated, and the purpose of clean production can be achieved.
Not purification directly making 2 - {(N - 4 - chlorophenyl) -3 - [...] methyl} nitrobenzene
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Paragraph 0012; 0013, (2018/07/30)
Without purification directly making 2 - {(N - 4 - chlorophenyl) - 3 - methyl pyrazole oxygen radical} nitrobenzene method, steps of the method are: in the reactor of the 1 - (4 - chlorophenyl) - 3 - after the end of the reaction the pyrazole is mellow, will be made before O-nitryl phenmethyl bromine a batch of all input to the 1 - (4 - chlorophenyl) - 3 - in the pyrazole is mellow solution, adding an amount of the sodium hydroxide solution, adjusting PH=13 above; and then to the reaction kettle is added 4 butyl ammonium bromide catalyst 0.2 kg, raising the temperature to 80 °C -82 °C, thermal insulation 2 hours, still 1 hours, layered, cooling to 0 - 5 °C; congeals the centrifugal separation, inlet dryer drying, to obtain the finished product 2 - {(N - 4 - chlorophenyl) - 3 - [...] methyl} nitrobenzene. This method avoids the acid neutralization, thermal insulation, the drying procedure, save the material repeatedly turnover, shorten the reaction time, the process is simple, easy to operate, the production efficiency is high; without the loss of the material in the production process, high yield; sewage and low emission, and protect the environment.
Synthetic process of 2-[N-4-chlorphenyl-1H-pyrazole-yloxymethyl] nitrobenzene
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Paragraph 0027; 0028; 0029; 0030; 0031; 0032; 0033-0043, (2017/08/29)
The invention discloses a synthetic process of 2-[N-4-chlorphenyl-1H-pyrazole-yloxymethyl] nitrobenzene. The synthetic process comprises the following steps: 1) putting solid 1-(4-chlorphenyl)-3-pyrazolol into a condensation kettle containing an O-nitrobenzyl bromobenzene solution; 2) raising the temperature and dropwise adding a sodium hydroxide aqueous solution; 3) cooling to a room temperature after the end of dropwise adding and then performing heat preservation for 1-2 hours, crystallization and centrifugation; 4) putting an obtained centrifugal solid into a refining kettle for refining; 5) putting methanol into the refining kettle for temperature rise and backflow; 6) cooling a material in the refining kettle to a room temperature and then performing heat preservation, crystallization and centrifugation; 7) centrifuging the solid and drying to obtain a pure product, namely the 2-[N-4-chlorphenyl-1H-pyrazole-yloxymethyl] nitrobenzene. The synthetic process disclosed by the invention has the benefits that the process can be simplified, the period is short, and generated wastewater is less.
Method for synthesizing pyraclostrobin intermediate
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, (2017/01/17)
The invention discloses a method for synthesizing a pyraclostrobin intermediate. The synthetic method comprises the following steps: preparing an intermediate 1-(4-chlorophenyl)-3-hydroxy-1-h-pyrazole from 4-chlorophenylhydrazine hydrochloride prepared with p-bromochlorobenzene and hydrazine hydrate as reaction raw materials; reacting o-nitrotoluene with chlorine in the presence of a catalyst so as to prepare o-nitrobenzyl chloride; and subjecting 1-(4-chlorophenyl)-3-hydroxy-1-h-pyrazole and o-nitrobenzyl chloride to an etherification reaction so as to obtain the pyraclostrobin intermediate, i.e., an etherification product 2[(N-4-chlorophenyl)-3-pyrazolyl-oxymethyl]nitrobenzene. The synthetic method provided by the invention can greatly reduce the amount of waste water produced in the synthesis process of 4-chlorophenylhydrazine hydrochloride; with 4-chlorophenylhydrazine hydrochloride as a raw material, the produced intermediate 1-(4-chlorophenyl)-3-hydroxy-1-h-pyrazole has HPLC content of no less than 98% and yield of no less than 90%; since chlorine is used for replacing bromine or hydrobromic acid to prepare o-nitrobenzyl bromide, production cost and environmental protection burden are controlled; and the etherification product with a content of no less than 98% and yield of no less than 90% is obtained.
Ortho-nitro benzyl chloride by a synthetic method of preparing pyraclostrobin intermediate (by machine translation)
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Paragraph 0063, (2016/10/31)
This invention relates to a kind of the ortho-nitro benzyl chloride preparation pyraclostrobin method for synthesizing intermediate, comprising the following steps: in the ortho-nitro toluene, a catalyst is added, heating and stirring, and slowly inject chlorine, after the end of reaction, recovering O-nitro-toluene, ortho-nitro benzyl chloride obtained; the ortho-nitro benzyl chloride and 1 the [...] (the 4 [...] chlorolphenyl) - 3 the the pyrazole is mellow[...] for etherification reaction, to obtain the 2 [...] [(N -4 the [...] chlorolphenyl) - 3 the pyrazole oxygen radical[...] methyl] nitrobenzene. In this invention to replace nitryl chlorine animal pennitryl bromination animal pen and adjacent to the 1 [...] (the 4 [...] chlorolphenyl) - 3 the reaction the pyrazole is mellow[...], pyraclostrobin intermediates prepared by the 2 [...] [(N -4 the [...] chlorolphenyl) - 3 the pyrazole oxygen radical[...] methyl] nitrobenzene, avoid the use of a defect method for synthesis of O- nitryl bromination animal pen, content can be used for preparing ≥ 98%, yield ≥ 90% ether product. (by machine translation)
