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82 results about "Picoline" patented technology

Picoline refers to any of three isomers of methylpyridine ([[carbon|CH₃C₅H₄N. They are all colorless liquids with a characteristic smell similar to that of pyridine. They are miscible with water and most organic solvents.

Bismuth-rich metal organic framework antibacterial material and preparation method thereof

The invention discloses an antibacterial material rich in a bismuth metal organic framework and a preparation method thereof, the method comprises the following steps: adding an indole monomer and an alcohol monomer into a solvent, and then adding nitrosalicylaldehyde into the solvent to obtain a spiropyran compound; the preparation method comprises the following steps: adding humic acid into a binary solvent consisting of dioxane and butanol to obtain a mixed solution; the ratio of the mass of the humic acid to the volume of the binary solvent is (2-3): (20-40) g / ml; sequentially adding a bismuth source, 2-bromo-5-(trifluoromethyl) pyridine and 4-(trifluoromethyl) phenylboronic acid into the mixed solution to obtain a bismuth metal organic framework; and adding the spiropyran compound into the bismuth metal organic framework to obtain the antibacterial material rich in the bismuth metal organic framework. The antibacterial capability of the antibacterial material is improved.
Owner:NINGBO FOTILE KITCHEN WARE CO LTD

Green preparation method of fluopyram intermediate 3-chloro-5-(trifluoromethyl)-2-ethylaminopyridine

The invention relates to a green preparation method of fluopyram intermediate 3-chloro-5-(trifluoromethyl)-2-ethylaminopyridine, which comprises the following steps: step 1, Ullmann reaction: coupling 3-chloro-2-methyl-5-trifluoromethylpyridine (C1) and N-bromomethyl phthalimide (C2) in the presence of a copper catalyst and potassium tert-butoxide to generate an intermediate (C3); and step 2, hydrolysis reaction: hydrolyzing the intermediate (C3) in the presence of hydrazine sulfate and an alkaline condition to generate the fluopyram intermediate 3-chloro-5-(trifluoromethyl)-2-ethylamino pyridine. The method has the advantages of short synthesis steps, easily available raw materials, no use of high-toxicity cyanogen compounds, low catalyst cost, difficult poisoning, recycling, simple post-treatment process, and less waste liquid generation, greatly reduces the production cost, improves the production safety, reduces the waste liquid discharge amount, and accords with the idea of green synthesis.
Owner:利民化学有限责任公司

A preparation method of beta-methylenepyridine-2-ethanol

The present invention relates to a preparation method of beta-methylenepyridine-2-ethanol. The preparation method of beta-methylenepyridine-2-ethanol uses 2-picoline as a first raw material, formaldehyde solution or paraformaldehyde as a second raw material, and urotropine as a catalyst, and reacts according to the following steps: (1) the first raw material, the second raw material, the catalyst and water are mixed and placed in an autoclave, the temperature is raised to 140-160° C., and after reacting for 18-20 hours, a solution containing beta-methylenepyridine-2-ethanol is obtained; (2) the solution containing beta-methylenepyridine-2-ethanol is distilled to obtain a product. The present application uses urotropine as a catalyst, utilizes its unique spatial structure and charge distribution, improves the selectivity of the reaction, and the reaction process is solvent-friendly, the steps are simple, and beta-methylenepyridine-2-ethanol can be obtained by a one-pot method, which is suitable for industrialization.
Owner:FUYANG XINYIHUA PHARM TECH CO LTD

Preparation method of novel bactericide fluoride ether bacteria amide

The invention provides a preparation method of fluoride ether bacteria amide, which comprises the following steps: dissolving pentafluorobenzonitrile in a solvent, dropwise adding a sodium methoxide solution at-10-30 DEG C for 2-15 hours, continuing to carry out heat preservation reaction for 0.5-2 hours after dropwise adding, and carrying out post-treatment to obtain 2, 3, 5, 6-tetrafluoro-4-methoxybenzonitrile; the preparation method comprises the following steps: jointly dissolving 2, 3, 5, 6-tetrafluoro-4-methoxybenzonitrile, 3-chloro-5-(trifluoromethyl) pyridine-2-yl) methanol and a catalyst acid in a solvent, reacting at 50-110 DEG C for 5-32 hours, and performing post-treatment on the obtained reaction liquid to obtain fluoride ether bacteria amide, according to the method, sodium methoxide and pentafluorobenzonitrile which are low in price and easy to obtain are subjected to etherification reaction, thionyl chloride and bis (trichloromethyl) carbonate are not used, the green chemical principle is met, and the method has the advantages of being short in step, safe and easy to operate and the like, so that the method has high implementation value and practical production applicability.
Owner:ZHEJIANG UNIV OF TECH

Near-infrared absorption zwitterionic ethylene-linked covalent organic framework photocatalyst as well as preparation method and application thereof

The invention discloses a near-infrared absorption zwitter-ion ethylene-linked covalent organic framework photocatalyst as well as a preparation method and application thereof, and the preparation method comprises the following steps: carrying out hydrothermal reaction on a mixture of an N-(3-sulfopropyl)-2, 4, 6-(trimethyl) pyridine monomer, an aldehyde monomer containing a thiophene unit, organic alkali and water to obtain the near-infrared absorption zwitter-ion ethylene-linked covalent organic framework photocatalyst. The zwitterionic ethylene-linked covalent organic framework photocatalyst ZVCOFs with near-infrared absorption is obtained. According to the method, a one-step green hydrothermal method is adopted, water is used as a solvent, pollution to the environment is reduced, traditional tedious freezing-pumping-unfreezing operation is omitted, high-yield COFs are obtained, and the method has the potential of industrial amplification. The ZVCOFs show excellent hydrophilicity due to rich zwitterionic groups and thiophene units, the light absorption range can be expanded to a near-infrared light region, the light absorption band edge reaches up to 852-1230 nm, and the ZVCOFs have excellent hydrogen evolution performance of photocatalytic water decomposition.
Owner:XI AN JIAOTONG UNIV

Process for the production of 4-amino-5-methyl-(1H)-pyridin-2-one and derivatives

An improved process for the production of 4-amino-5-methyl-(1H)-pyridin-2-one and derivatives. In the process, 4-hydroxy-5-methyl-(1H)-pyridin-2-one is reacted under pressure with an ammonium salt without adding aqueous ammonia or feeding in gaseous ammonia to provide the target compounds in high yield and high purity. The reaction mixture is not or much less corrosive to enamel coatings of a reaction container surface, since gaseous ammonia as reagent is not used.
Owner:MINASCENT TECHNOLOGIES GMBH

A trifluoromethyl pyridine derivative, its preparation method and use

The application provides a trifluoromethyl pyridine derivative and a preparation method and application thereof, and belongs to the technical field of organic synthesis; the trifluoromethyl pyridine derivative is constructed by using a trifluoromethyl α,β‑ unsaturated imine, the trifluoromethyl pyridine derivative emits blue fluorescence at a wavelength of 300-500 nm, has good optical properties and good bacteriostatic activity, is expected to be used in the fields of organic light-emitting materials and pesticides, and has a wide application prospect; the preparation method is simple and fast, has a wide substrate range, uses cheap and easily available raw materials, and does not cause environmental pollution; the preparation method of the trifluoromethyl pyridine derivative has the advantages of simple process, high yield and good universality, and has good practicability.
Owner:SHIHEZI UNIVERSITY

Composite catalyst, preparation method thereof and application of composite catalyst in synthesis of 2-methylpyridine

The invention discloses a composite catalyst as well as a preparation method and application thereof in synthesis of 2-methylpyridine, and belongs to the technical field of chemical synthesis. The composite catalyst is prepared by adopting an ultrasonic-coprecipitation method: dissolving nickel salt into a 0.01-1mol / L solution, slowly adding a precipitant solution for precipitation, and then performing aging, ultrasonic treatment, filtration, washing and drying, calcination and hydrogen reduction. When the catalyst is applied to synthesis of 2-methylpyridine, pyridine is taken as a main raw material, methanol is taken as an auxiliary raw material, a reaction is carried out in a fixed bed under the conditions that the temperature is 170-300 DEG C, the pressure is 0.7-1.8 MPa and the air speed is 0.5-3h <-1 >, and a high-purity product is obtained after a crude product is rectified. The catalyst is uniform in active component distribution, recyclable and mild in reaction condition, the yield of the 2-methylpyridine product reaches 51%, the purity exceeds 99%, the cost is reduced, and industrial chain extension is facilitated.
Owner:TAIAN MINGDE NEW MATERIALS CO LTD

Preparation method of sulfoxaflor

According to the preparation method of sulfoxaflor, provided by the invention, 3-[1-(methylthio) ethyl]-6-(trifluoromethyl) pyridine is taken as a raw material, and is subjected to an S-imidization reaction in the presence of DPPH and an ionic liquid [Bmin] BF4 to prepare a sulfimide compound B; the sulfoxaflor is finally prepared through an N-cyanation reaction of the sulfoxaflor compound B and AIBN in the presence of cuprous iodide, potassium carbonate and [Bmin] BF4, the preparation method of the sulfoxaflor is short in synthesis route, the ionic liquid is creatively used as the reaction solvent, the sulfoxaflor is more environmentally friendly, the reaction can be promoted, and the preparation method of the sulfoxaflor is suitable for industrial production. The reaction time is shortened, and the target product can be prepared with high yield (the total yield of two steps is 81% or above) and high purity (99.5%).
Owner:GUANGDONG JINDU BIOTECHNOLOGY CO LTD

Method for directly reducing carboxylic acid into aldehyde

The invention relates to the technical field of compound synthesis, in particular to a method for directly reducing carboxylic acid into aldehyde. The preparation method comprises the following steps: mixing triphenylphosphine, dichloromethane, carboxylic acid and N-chlorosuccinimide, and reacting to obtain a reactant; mixing with pinacol borane and 4-dimethyl pyridine, and continuously reacting to obtain a continuous reactant; and separating and purifying to obtain aldehyde. The synthesis of the substrate carboxylic acid provided by the invention and the rapid deoxidation of the carboxylic acid are carried out to obtain an aldehyde product, especially the following compounds 2aa, 2ab, 2ae, 2bc, 2be, 2bf, 2bg, 2bh, 2bi, 2bj, 2bk and 2bl have catalytic hydrolysis effects on hypophosphamide; the compound 2bl has a particularly excellent effect on hydrolysis of hypophosphamide.
Owner:GUIZHOU UNIV

Antibacterial agent for hard surface and preparation method thereof

The invention discloses an antibacterial agent for a hard surface and a preparation method of the antibacterial agent, and relates to the technical field of disinfection and sterilization. When the antibacterial agent for the hard surface is prepared, silicon dioxide sequentially reacts with chloropropyltriethoxysilane, 2, 2 '-dimethyl pyridine amine and zinc nitrate to prepare modified silicon dioxide; the preparation method comprises the following steps: reacting phytic acid with 3-butene-1-amine to obtain modified phytic acid; the preparation method comprises the following steps: reacting polyvinyl alcohol with 4-chloropropionic acid and N-allylimidazole in sequence to prepare modified polyvinyl alcohol; and uniformly mixing the modified polyvinyl alcohol, the modified phytic acid, the modified silicon dioxide, azodiisobutyronitrile, absolute ethyl alcohol and deionized water to prepare the antibacterial agent for the hard surface. The prepared antibacterial agent for the hard surface has excellent antibacterial performance and wear resistance.
Owner:SICHUAN RONGCHENG XINYUAN TECH CO LTD

Preparation method of N-(5-pyrimidinemethyl)-2-pyridylamine

ActiveCN120842201AOrganic chemistryPalladium on carbonPtru catalyst
The invention relates to a preparation method of a heterocyclic compound, in particular to a preparation method of N-(5-pyrimidinemethyl)-2-pyridylamine, which comprises the following steps: (1) reacting 4, 6-dihydroxypyrimidine with N, N-dimethylformamide and phosphorus oxychloride at 20-30 DEG C for 0.5-1 hour, heating to 110-115 DEG C, and reacting for 3-4 hours to obtain 4, 6-dichloropyrimidine-5-formaldehyde; (2) reacting the 4, 6-dichloropyrimidine-5-formaldehyde with a palladium carbon catalyst and a metal salt synergistic catalyst in a hydrogen atmosphere at 40-50 DEG C for 5-6 hours to obtain 5-hydroxymethyl pyrimidine; (3) reacting the 5-hydroxymethylpyrimidine with methylsulfonyl chloride at the temperature of-5 to 5 DEG C to obtain pyrimidine-5-methyl methanesulfonate; and (4) enabling the pyrimidine-5-methyl methanesulfonate to react with 2-aminopyridine for 4 hours at the temperature of 50 to 60 DEG C, so as to obtain the N-(5-pyrimidinemethyl)-2-pyridylamine.
Owner:ZHEJIANG WEIFENG PHARM CO LTD

Method for green synthesis of fluopyram through one-pot method

The invention belongs to the field of fluorine-containing pesticide synthesis, and particularly relates to synthesis of fluopyram. The fluopyram is innovatively synthesized by adopting a one-pot catalytic system, and the reaction process is as shown in the formula 1: 2-acetonitrile-3-chloro-5-trifluoromethylpyridine (1) and o-trifluoromethyl benzoyl chloride (2) are used as initial raw materials, a catalyst with a specific structure and an alkali-binding acid agent are added into an ionic liquid, and a reaction is performed at the temperature of 60-80 DEG C for 1-2 hours to obtain the fluopyram. And preparing the target product fluopyram (3) by a high-efficiency one-pot method under the catalytic action of a supported metal catalyst in a hydrogen atmosphere. According to the one-pot synthesis process of fluopyram, the reaction is clean and pollution-free, the operation is simple and convenient, the utilization rate of raw materials is high, and the application frequency of Raney nickel can be increased under the condition that the yield is not influenced through a reaction system formed by combining water and an organic solvent. The o-trifluoromethyl benzoic acid recovered from the water phase can be further converted into o-trifluoromethyl benzoyl chloride, so that the utilization rate of the raw materials is improved. The synthesis process route is effectively shortened, and meanwhile, the use of expensive protection groups for protection in the hydrogenation reduction process is avoided, so that the process is more simplified.
Owner:NANJING TECH UNIV

Synthetic method of indoloquinazolinone compound

The invention relates to a synthetic method of an indoloquinazolinone compound. The synthetic method comprises the following steps: reacting 2-aminoacetophenone with aryl isocyanate under the catalytic action of a palladium complex to obtain the indoloquinazolinone compound, wherein the palladium complex is an N, N-coordinated palladium complex containing a meta-carborane ligand. The preparation process of the palladium complex comprises the following steps: adding an n-BuLi solution into a meta-carborane solution to carry out a deprotonation reaction, then adding 3-chloromethylpyridine to carry out a nucleophilic substitution reaction, finally adding Pd (OAc) 2 to carry out a coordination reaction to obtain a palladium complex head product, and carrying out post-treatment to obtain the palladium complex product. Compared with the prior art, the method disclosed by the invention has the advantages of good adaptability, high catalytic efficiency, few byproducts, mild reaction conditions, lower cost, easiness in product separation, no generation of a large amount of waste residues and the like.
Owner:SHANGHAI INST OF TECH

Method for simultaneously preparing cyantraniliprole metabolites IN-JCZ38 and IN-J9Z38

The invention relates to a method for simultaneously preparing cyantraniliprole metabolites IN-JCZ38 and IN-J9Z38, and belongs to the technical field of pesticide metabolites. The method comprises the following steps: (1) taking cyantraniliprole as a raw material, and generating a metabolite IN-JCZ38 and a byproduct under the action of H2O2 and alkali; (2) generating a metabolite IN-J9Z38 from the by-product under the action of a dehydrating agent and a catalyst; the alkali is one of sodium hydroxide, sodium carbonate or sodium bicarbonate; the catalyst is one of N, N-dimethyl formamide, pyridine or 3-methylpyridine. The preparation method disclosed by the invention is high in raw material utilization rate and simple in synthesis method, realizes continuous reaction and byproduct reutilization, can be used for simultaneously preparing two metabolites, is beneficial to large-scale preparation of cyantraniliprole metabolites, and meets the demand of cyantraniliprole metabolite samples in pesticide registration toxicology detection.
Owner:SHANDONG YISHENG IND CO LTD

Low self-discharge supercapacitor electrolyte, preparation method and application thereof

ActiveCN121545927BElectrolytic agentMeth-
The application provides a supercapacitor electrolyte with low self-discharge, a preparation method and application thereof, raw materials of the supercapacitor electrolyte include organic solvents, ammonium salt and pyridine oxide; the organic solvents are one or more of acetonitrile, fluoroacetonitrile, propionitrile, butyronitrile and isobutyronitrile; the ammonium salt is tetraethylamine bistrifluoromethylsulfonylimide or tetraethylammonium bis(trifluoromethanesulfonyl)imide; and the pyridine oxide is pyridine-N-oxide, 4-methylpyridine oxide or 3-methylpyridine oxide. By selective use of specific additives and optimized configuration of electrolyte salt, the supercapacitor electrolyte of the application can effectively reduce the self-discharge rate of the supercapacitor and significantly improve the energy utilization efficiency of the capacitor.
Owner:XIAN XD POWER CAPACITOR CO LTD +1

Organic photocatalytic material and preparation method thereof

The application relates to the technical field of catalytic materials, and relates to an organic photocatalytic material and a preparation method thereof.1, comprising the following steps: mixing modified N-hydroxy phthalimide phenylacetate, an aliphatic nitroalkane, 2,6-dimethylpyridine, a photocatalyst and a solvent, then irradiating under visible light, placing in an inert atmosphere, stirring for 2-8 hours, and obtaining a product through post-treatment to obtain a final product; the mass ratio of the modified N-hydroxy phthalimide phenylacetate, the nitro compound, the 2,6-dimethylpyridine, the photocatalyst and the solvent is 2-5:1-2:1-3:1:8-11. The visible light catalysis method can be used to synthesize the nitro compound under mild conditions, and further provides a green and efficient new path for the preparation of a nitrogen-containing drug intermediate.
Owner:DEZHOU UNIV

Preparation method of tovorafenib intermediate

The invention discloses a preparation method of a tovorafenib intermediate, and belongs to the field of organic synthesis. The tovorafenib intermediate is (R)-2-(1-aminoethyl)-N-(5-chloro-4-(trifluoromethyl) pyridine-2-yl) thiazole-5-carboxamide, and the method mainly comprises the following steps: dissolving 2-acetyl-N-(5-chloro-4-(trifluoromethyl) pyridine-2-yl) thiazole-5-carboxamide in a solvent, adding p-toluenesulfonic acid, dropwise adding S (-)-alpha-phenylethylamine for reaction, and carrying out column chromatography separation to obtain the tovorafenib intermediate. Recovering the solvent from the product to obtain an oily intermediate; then dropwise adding S (-)-alpha-phenylethylamine, and adding DBU for reaction; and after the reaction is finished, carrying out reduced pressure distillation to recover the S (-)-alpha-phenylethylamine, so as to obtain an oily substance, adding water into the oily substance, and crystallizing, so as to obtain the tovorafenib intermediate. According to the method, S (-)-alpha-phenylethylamine is used as a reactant and a chiral inducer at the same time, p-toluenesulfonic acid is used as a condensation catalyst, and DBU is used for catalyzing epimerization; the theoretical 100% yield is achieved through high-temperature racemization.
Owner:HANGZHOU YOUHUA BIOTECHNOLOGY CO LTD

Absorption liquid with high cycle stability for capturing carbon dioxide as well as preparation method and application of absorption liquid

The invention discloses a high-cycle-stability absorption liquid for capturing carbon dioxide and a preparation method and application thereof, and relates to the technical field of gas separation and purification, the absorption liquid comprises a main absorption component, an auxiliary absorption component, an active component, an additive and a solvent; the additive is 4, 4 '-dihydroxy diphenyl ether and 3-methyl-3H-imidazole methyl [4, 5-b] pyridine-6-carboxylate; the solvent is water. The absorption liquid provided by the invention can be used for capturing carbon dioxide in industrial waste gas, has excellent carbon dioxide absorption and desorption capacity and rapid absorption and desorption kinetics, improves the CO2 absorption load capacity, has excellent absorption and desorption rate and low-temperature capturing performance, and has better stability in long-period operation. In addition, the method solves the problems of cost, energy consumption, environment compatibility and the like, and has a good application prospect.
Owner:DEPP DRY ICE MFG (DALIAN) CO LTD +1

Method for determining potential genotoxic impurities in esomeprazole sodium by HPLC (High Performance Liquid Chromatography)

PendingCN120609923AComponent separationOmeprazole SodiumEsomeprazole Sodium
The invention discloses a method for determining potential genotoxic impurities in esomeprazole sodium by HPLC (High Performance Liquid Chromatography), which comprises the following steps: preparing a test solution: taking 20-100mg of esomeprazole sodium, precisely weighing, putting into a 10mL measuring flask, adding methanol, carrying out ultrasonic treatment to dissolve a sample, diluting to a scale by using methanol, and shaking uniformly; a proper amount of 4-methoxy-3, 5-dimethyl pyridine nitrogen oxide is taken, precisely weighed and quantified with methyl alcohol, and the reference substance solution containing 73-360 ng of 4-methoxy-3, 5-dimethyl pyridine nitrogen oxide in 1 mL of the solution is prepared; respectively carrying out HPLC (High Performance Liquid Chromatography) detection on the reference substance solution and the test solution, and determining the content of the impurity 4-methoxy-3, 5-dimethyl pyridine nitrogen oxide in the esomeprazole sodium by adopting an external standard method. The method has the advantages of high separation efficiency, high analysis speed, high detection sensitivity and low detection cost, and can effectively control the quality of esomeprazole sodium.
Owner:南京红太阳医药研究院有限公司

A mxene aerogel separator and a preparation process thereof

The application discloses an MXene aerogel diaphragm and a preparation process thereof, and belongs to the technical field of lithium battery diaphragms. The MXene aerogel diaphragm disclosed by the application contains the following components in parts by weight: 100 parts of modified carboxymethyl cellulose, 5-15 parts of MXene nanosheets, 20-30 parts of a crosslinking agent, 0.1-100 parts of a pH regulator, and 10000-20000 parts of a solvent. The modified carboxymethyl cellulose is prepared by first subjecting sodium carboxymethyl cellulose to a nucleophilic ring-opening reaction with glycidyl methacrylate to obtain GMA-CMC, and then subjecting the GMA-CMC to a Michael addition with 2-amino-4-(trifluoromethyl) pyridine hydrochloride. The MXene aerogel diaphragm disclosed by the application has excellent structural stability, high ionic conductivity and good thermal stability.
Owner:WEIWEI (GUANGDONG) NEW MATERIAL TECHNOLOGY CO LTD

A method for synthesizing seven-membered ring ether compounds

The present invention discloses a method for synthesizing a seven-membered cyclic ether compound, comprising the following steps: (1) reacting 2,4,6-trimethylpyridine nitrogen oxide with an alkyl p-toluenesulfonate in the presence of a solvent to obtain pyridine nitrogen oxide p-toluenesulfonate; and (2) subjecting pyridine nitrogen oxide p-toluenesulfonate to a cycloaddition reaction with a conjugated diene compound in the presence of a photocatalyst and a solvent under visible light irradiation to obtain the seven-membered cyclic ether compound. The above-mentioned synthesis method is simple to operate, has mild reaction conditions, requires a small amount of catalyst for the reaction, is time-consuming, and the product is easy to purify, making it suitable for industrial mass production. In addition, the reaction substrate of the synthesis method has wide applicability, and a seven-membered cyclic ether compound with multiple substituents can be designed and synthesized according to demand.
Owner:SUZHOU UNIV

A method for synthesizing picoxystrobin

PendingCN122277467AMeth-Organic synthesis
This invention relates to a method for synthesizing azoxystrobin, belonging to the field of organic synthesis technology. The method uses 2-(2-(chloromethyl)phenyl)-3-methoxyacrylonitrile and 2-hydroxy-6-trifluoromethylpyridine as raw materials, condensing them under alkaline conditions to obtain an etherified intermediate, which is then directly hydrolyzed and esterified with methanol under acidic conditions to obtain azoxystrobin. This method avoids the use of expensive 3-isochloroketone as a raw material, using inexpensive 2-(2-(chloromethyl)phenyl)-3-methoxyacrylonitrile prepared from o-methylphenylacetonitrile as the key fragment, further reducing the cost of azoxystrobin raw materials. Furthermore, the process route is simple, the yield is high, and it is suitable for industrial production.
Owner:LIAONING ZHONGHUI BIOTECHNOLOGY CO LTD

Crystalline form a of GLP-1 receptor agonist and preparation method therefor

PendingUS20260200933A1Propanoic acidIsoquinoline
The invention relates to a crystal form A of(S)-2-(3S,8S)-3-(4-(3,4-dichlorobenzyloxy)phenyl-7-((S)-1-phenylpropyl)-2,3,6,7,8,9-hexahydro-[1,4]-dioxino[2,3-g]isoquinolin-8-ylformylamino)-3-(4-(2,3-dimethylpyridin-4-yl)phenyl)propionic acid (“OAD2”), and methods of preparation thereof. Crystal form A may be useful in the treatment of various conditions and metabolic disorders including, but not limited to, type 2 diabetes.
Owner:HANGZHOU ZHONGMEI HUADONG PHARMACEUTICAL CO LTD

A process for the preparation of fluopyram

The application discloses a preparation method of fluopyram, which comprises the following steps: step 1: in the presence of solvent 1 and a base, dimethyl malonate and 2,3-dichloro-5-trifluoromethyl pyridine are added to react, a salt reaction is carried out by adjusting pH, and 2-[3-chloro-5-(trifluoromethyl) pyridyl] dimethyl malonate potassium salt, namely intermediate 1, is obtained; step 2: o-trifluoromethyl benzoyl chloride, an organic base and chloromethylamine are added to react, and intermediate 2 is obtained; step 3: solvent 3, intermediate 1 and intermediate 2 are added to react, and intermediate 3 is obtained; step 4: water, a base, solvent 4 and intermediate 3 are added, pH is adjusted after reaction, and continuous reaction is carried out, and fluopyram is obtained. By adopting the preparation method, the yield of fluopyram is high, the purity is high, the reaction time is short, the reaction condition is mild, and the method is suitable for mass production.
Owner:YIFAN BIOTECHNOLOGY (SHANGHAI) CO LTD

Method for obtaining 2,3-diphenyl-6-{[5-(trifluoromethyl)pyridine-2-yl]oxy}-6,7-dihydro-5h-imidase[2,1-b][1,3]thiazine

Method for obtaining 2,3-diphenyl-6-{[5-(trifluoromethyl)pyridine-2-yl]oxy}-6,7-dihydro-5H-imidase[2,1-b][1,3]thiazine involves the reaction of starting material, 6-hydroxy-2,3-diphenyl-6,7-dihydro-5H-imidase[2,1-b][1,3]thiazine, with halogen-substituted pyridine in dimethylformamide. Previously obtained solution of 2,3-diphenyl-6,7-dihydro-5H-imidazo[2,1-b] [1,3]thiazine-6-ol and NaH in dimethylformamide is stirred for 0.5 hours at room temperature; only then is 5-(trifluoromethyl)-2-chloropyridine added in a 1:1 ratio, and mixture is subjected to intensive stirring for 24 hours. Then reaction mixture is poured onto ice; resulting precipitate is filtered off and identified as 2,3-diphenyl-6- {[5-(trifluoromethyl)pyridin-2-yl]oxy}-6,7-dihydro-5H-imidazo[2,1-b][1,3]-thiazine. Thus, the synthesis is carried out by first preparing solution of starting compound with NaH using the method of prolonged stirring, followed by the main synthesis with a reaction time of 24 hours.
Owner:LESYA UKRAINKA VOLYN NATIONAL UNIVERSITY

Green synthesis process of 2-amino-3-chloro-5-trifluoromethylpyridine

PendingCN120887829AOrganic chemistryTrifluoromethylationPtru catalyst
The invention discloses a green synthesis process of 2-amino-3-chloro-5-trifluoromethylpyridine, and belongs to the technical field of preparation of pesticide intermediates. The method comprises the following steps: by taking 3, 5-dichloropyridine as a raw material, carrying out nitrogen-oxidation reaction; then carrying out trifluoromethylation reaction under the action of a palladium catalyst; then carrying out chlorination reaction on phosphorus oxychloride; and finally, carrying out ammonification reaction to generate the 2-amino-3-chloro-5-trifluoromethylpyridine. According to the method, all the raw materials can be conveniently purchased on the market, the process of each step of reaction is simple and convenient, chloropyridine is directly subjected to trifluoromethylation by adopting trifluoromethyl potassium trifluoroborate and a palladium catalyst, the reaction yield is high, and industrial production is easy; meanwhile, a by-product ammonia chloride generated in the mother liquor in the amino substitution step can be recycled as a by-product.
Owner:WUHAN INST OF TECH +2