102 results about "Picoline" patented technology

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.

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.

The invention provides a preparation method of picoxystrobin, and belongs to the technical field of bactericides. According to the preparation method of picoxystrobin, no intermediate needs to be separated in the preparation process, side reactions are few, production operation is simpler, the product yield and purity are high, and the preparation method is suitable for industrial production. And the etherification reaction raw material used in the invention is 2-chloro-6-trifluoromethylpyridine, has no large corrosivity or safety risk, is convenient for post-treatment, has low requirements on production equipment, and is lower in cost.

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.

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.

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.

The utility model belongs to the technical field of 2-chloro-5-chloromethylpyridine production equipment, and particularly relates to a 2-chloro-5-chloromethylpyridine continuous rectification mechanism which comprises a first rectification furnace, a feeding pipe is fixedly connected to the outer surface of the first rectification furnace, a liquid outlet is formed in the lower surface of the first rectification furnace, a funnel is fixedly connected to the lower surface of the first rectification furnace, and a liquid outlet is formed in the lower surface of the funnel. A first collecting box is fixedly connected to the lower surface of the funnel, a first pipeline is fixedly connected to the front side face of the first collecting box, a first infusion pump is fixedly connected to the other end of the first pipeline, and a second pipeline is fixedly connected to the upper surface of the first infusion pump. The 2-chloro-5-chloromethylpyridine extraction device disclosed by the utility model is reasonable in structure, can be used for re-extracting 2-chloro-5-chloromethylpyridine in waste liquid generated by rectification during use, improves the extraction rate of 2-chloro-5-chloromethylpyridine, reduces the loss of 2-chloro-5-chloromethylpyridine, and is beneficial to preparation of 2-chloro-5-chloromethylpyridine.

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.

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.

The invention discloses a synthesis method of 2, 3-dichloro-5-trifluoromethylpyridine, which comprises the following steps: mixing a copper catalyst, a ligand and alkali, then adding an organic solvent, 5-bromo-2, 3-dichloropyridine and trifluoromethyltrimethylsilane under the protection of inert gas, then heating and stirring until the reaction is complete, and after the reaction is complete, carrying out post-treatment to obtain the 2, 3-dichloro-5-trifluoromethylpyridine. The catalyst is 2, 3-dichloro-5-trifluoromethylpyridine. The method has the beneficial effects that the copper catalyst used in the method is cheap and easy to obtain, the raw materials are easy to obtain non-toxic substances, the process operation is simple, convenient and safe, the yield is good, the reaction solvent can be recycled and reused, a foundation is laid for further amplification, and a new method is provided for synthesizing the 2, 3-dichloro-5-trifluoromethylpyridine.

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.

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%).

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.

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.

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.

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.

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.

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.

The invention relates to the technical field of fine chemical engineering, and particularly discloses a purification method of a 2-chloro-5-chloromethylpyridine synthetic liquid, which mainly comprises the following steps: carrying out reduced pressure distillation on the 2-chloro-5-chloromethylpyridine synthetic liquid to remove toluene to obtain a distillation base solution; adding an extracting agent into the distillation base solution, extracting, standing for layering, and collecting supernatant to obtain an extracting solution; heating and distilling the extracting solution to remove the extracting agent, so as to obtain a 2-chloro-5-chloromethylpyridine crude product; and adding a calcium salt stabilizer into the 2-chloro-5-chloromethylpyridine crude product, and carrying out high-vacuum distillation to collect distillate, thereby obtaining the 2-chloro-5-chloromethylpyridine product. The 2-chloro-5-chloromethylpyridine product obtained by the purification method has the characteristics of high content, high yield and simple purification process, the extraction agent process is used for replacing hydrolysis and neutralization processes, the extraction agent can be recycled, no water is introduced, no large amount of wastewater is generated due to introduction of water, and the method is suitable for industrial production.

The present disclosure provides crystalline forms, solvates, and hydrates of (R)-5-fluoro-2-methyl-1-((R)-5-(pyridin-2-yl)-2,3-dihydro-1H-inden-2-carbonyl)indoline-6-sulfonamide and methods of preparation.

The invention belongs to the technical field of organic chemical synthesis, and relates to a synthesis method and application of 3-trifluoromethyl-2-pyridine sulfonamide. According to the synthesis method, an oxime ester compound derived from 3-trifluoromethyl-2-pyridine carboxylic acid, a sulfur dioxide reagent, an additive and a photocatalyst are subjected to a reaction in a solvent under the photocatalysis condition, and the 3-trifluoromethyl-2-pyridine sulfonamide is obtained. According to the method, the oxime ester compound derived from the 3-trifluoromethyl-2-pyridine carboxylic acid reacts with the sulfur dioxide reagent under the photocatalytic condition, then modification is further carried out, the corresponding 3-trifluoromethyl-2-pyridine sulfonamide can be efficiently constructed, the reaction steps are short, the conditions are mild, operation is easy, and substrate compatibility is good; the reaction post-treatment is convenient, an additional metal reagent is not needed, pyrimidulfuron-methyl can be conveniently and efficiently synthesized, and the method has wide pharmaceutical chemistry and industrial synthesis values.

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.

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.

The invention relates to the field of pyridine and particularly provides a catalyst for pyridine synthesis as well as a preparation method and application thereof. The catalyst for pyridine synthesis is prepared from the following raw materials in parts by weight: 2-10 parts of metal salt and / or metal oxide, 10-30 parts of molecular sieve, 1-5 parts of titanium dioxide, 5-20 parts of kaolin, 20-40 parts of alumina sol and 20-40 parts of water. The catalyst for pyridine synthesis is prepared from the metal salt and / or the metal oxide, the molecular sieve, the titanium dioxide, the kaolin, the aluminum sol and the water according to a specific ratio, so that the titanium modified catalyst is obtained, and the catalyst is good in catalytic performance and high in pyridine yield and can be used for catalyzing acetaldehyde and ammonia to obtain 2-methylpyridine and 4-methylpyridine.

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.

The invention relates to a synthesis method of an abesilib intermediate, which comprises the following steps of: performing Grignard reagent treatment on 3, 5-difluorobromobenzene serving as a raw material, and reacting with 2-fluoro-N-methoxy-N-methylacetamide to obtain 1-(3, 5-difluorophenyl)-2-fluoroethane-1-ketone; then, carrying out nitration reaction to obtain 1-(3, 5-difluoro-4-nitrophenyl)-2-fluoroethane-1-ketone; in the presence of hydrogen and a catalyst, carrying out hydrogenation reduction to obtain 1-(4-amino-3, 5-difluorophenyl)-2-fluoroethane-1-ketone; the preparation method comprises the following steps: introducing acetyl through acetyl chloride, and condensing with N, N-dimethylformamide dimethyl acetal to prepare (Z)-N-(4-(3-(dimethylamino)-2-fluoroacryloyl)-2, 6-difluorophenyl) acetamide; the preparation method comprises the following steps: carrying out cyclization on 2-fluoro-1-(4-fluoro-1-isopropyl-2-methyl-1H-benzimidazole-6-yl) prop-2-en-1-one and isopropylamine under an alkali condition to obtain an abesiril intermediate (Z)-3-(dimethylamino)-2-fluoro-1-(4-fluoro-1-isopropyl-2-methyl-1H-benzimidazole-6-yl) prop-2-en-1-one; and finally, under an alkaline condition, carrying out cyclization on the compound and N-(5-(4-ethyl-piperazine-1-yl methyl) pyridine-2-yl) guanidine nitrate to obtain abesilib.

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.

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.

The utility model relates to a condensing device for processing 2-chloro-5-chloromethylpyridine, which comprises a base, a condensing kettle fixedly connected to one side of the top of the base, a water tank fixedly mounted on the other side of the top of the base, and a controller fixedly mounted on the front surface of the water tank, the stirring mechanism comprises a servo motor fixedly mounted at the top of the condensation kettle, and an output shaft of the servo motor is fixedly connected with a rotating shaft extending into the condensation kettle. According to the condensing device for 2-chloro-5-chloromethylpyridine processing, a servo motor is started to work through a controller, the servo motor works to drive a rotating shaft to rotate, a raw material body in the condensing kettle can be fully stirred, a condenser and a booster pump are started to work through the controller, and the raw material body can be fully stirred; and condensation treatment can be conveniently conducted on the raw material body in the condensation kettle, the condensation production efficiency is effectively improved, and the advantages of being high in condensation efficiency and high in practicability are achieved.