49 results about "Bromoacetic acid" patented technology

The invention discloses a preparation method of 3, 4-difluoro-2-methoxyphenylacetic acid, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: reacting 2, 3-difluorophenol with 3, 4-dihydropyran under the action of sulfonic acid resin to generate an intermediate 2-(2, 3-difluorophenoxy) pyran; then lithiating, reacting with tert-butyl 2-bromoacetate, and performing acidolysis to obtain a 3, 4-difluoro-2-hydroxyphenylacetic acid intermediate; and finally reacting with a methylation reagent in the presence of alkali to generate the target compound 3, 4-difluoro-2-methoxyphenylacetic acid. The preparation method has the advantages that the route is overall reasonable, the preparation method comprises three steps, and a simple and effective new route is provided for the preparation of the 3, 4-difluoro-2-methoxyphenylacetic acid.

The invention provides a synthesis method of (3-hydroxyadamantane-1-methoxycarbonyl) difluoromethanesulfonate photoacid generator anions, and relates to a photoacid generator anion synthesis method of (3-hydroxyadamantane-1-methoxycarbonyl) difluoromethanesulfonate photoacid generator anions. The preparation method comprises the following steps: S1, uniformly mixing a solvent and difluorobromoacetic acid, then adding CDI, fully stirring, then adding 3-hydroxy-1-adamantane methanol, fully reacting, then adding bicarbonate, carrying out liquid separation to obtain an organic phase A, washing the organic phase A, and carrying out drying and spin-drying; s2, fully mixing the spin-dried substance with NaHCO3, Na2S2O4, acetonitrile and ultrapure water, then carrying out liquid separation to obtain an organic phase B, and carrying out drying and spin-drying on the organic phase B; and S3, dissolving the spin-dried substance in water, then adding an H2O2 solution, carrying out a full reaction, and then carrying out cooling and post-treatment so as to obtain the photoacid generator anions. According to the method, 3-hydroxy-1-adamantane methanol and difluorobromoacetic acid are used as reaction raw materials, esterification reaction is performed under the condition of adding CDI to obtain a first-step reaction intermediate, then acylation sulfonation and oxidation reaction are performed to obtain the target product photoacid generator anion, the reaction process is mild in condition, and the product purity is high.

The present invention belongs to the technical field of semiconductor materials, and discloses a polymer with alternating arrangement of perylene diimide and naphthalene diimide, and its preparation method and application. The preparation method of the polymer includes the following steps: mixing naphthalic anhydride, alkanolamine and an organic solvent, and reacting to obtain naphthalene diimide-diol; mixing naphthalene diimide-diol, bromoacetic acid, 4-dimethylaminopyridine, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and an organic solvent, and reacting to obtain naphthalene diimide-dibromide; mixing naphthalene diimide-dibromide, perylene diimide-diamine and an organic solvent, and reacting to obtain the polymer. The present invention takes naphthalene diimide and perylene diimide as the core structures, and through design and synthesis, obtains a polymer with good water and alcohol solubility. This polymer can integrate the physical and chemical properties of the above two structural units, providing a guarantee for its application as an electron transport layer material in solar cells.

The invention discloses a nickel-cobalt hydrometallurgy circulation process, and relates to the technical field of hydrometallurgy. On one hand, magnesium sulfate solution wastewater is converted into magnesium salt liquid to replace sodium hydroxide to be saponified with an organic phase, and meanwhile water for a production line can be saved. Carbon dioxide waste gas is recycled, and industrial waste gas resource conversion and reuse are achieved. On the other hand, high-efficiency recovery of cobalt and nickel in the waste liquid is realized by preparing a functional material: a resin filtering membrane with a coordination trap on the surface is formed by virtue of Zn < 2 + > coordination activation, and cobalt and nickel ions in the waste liquid are efficiently captured; the preparation method comprises the following steps: pre-synthesizing a dimethyl glyoxime functional ligand with carboxyl by taking dimethylglyoxime and bromoacetic acid as raw materials, and directly constructing MOF (Metal Organic Framework) with a dimethyl glyoxime group for chelating Ni < 2 + >; the prepared adsorption particles are subjected to secondary adsorption in waste liquid after passing through resin, so that cobalt and nickel ions in the waste liquid reach an extremely high recovery rate. The hydrometallurgy can achieve the effect of neither recovery nor circulation.

The invention relates to the technical field of oil-water well sand consolidation agents, and discloses a modified resin and a preparation method and application thereof.The preparation method comprises the steps that diethanol amine, butyric acid and the like are subjected to a reaction, and a modifier is obtained; and reacting with bromoacetate phenolic resin to obtain the modified resin. The modified resin contains quaternary ammonium salt cation groups which can form electrostatic interaction with negative charges on the surface of sand, and meanwhile, the modified resin contains a large number of ester groups and amido bonds which form hydrogen bond interaction with hydroxyl on the surface of sand, so that the bonding strength between phenolic resin and sand is improved; the phenolic resin has better cementing and curing performance, inorganic materials such as nano silicon dioxide and nano boron nitride do not need to be added, the compressive strength of a cemented rock core sample is remarkably improved, and the phenolic resin has good practical application in an oil-water well sand consolidation agent.

The invention belongs to the field of organic chemistry, and particularly relates to a synthesis method of a rosuvastatin calcium key intermediate, which comprises the following steps: (1) taking (S)-4-chloro-3-hydroxybutyric acid as a raw material, and performing condensation ester with methanol under the condition of an esterification reaction condensing agent to obtain a compound with a structural formula B, and (2) taking the compound with the structural formula B as a raw material, and under the alkaline condition, performing condensation ester reaction to obtain the rosuvastatin calcium key intermediate. The preparation method comprises the following steps: (1) carrying out a reaction with tert-butyl malonate to obtain a compound with a structural formula C, (3) adding glucose and alkali into the compound with the structural formula C as a raw material under an enzyme catalysis condition to obtain a chiral reduction product D, and (4) heating the compound with the structural formula D as a raw material in the presence of only 2, 2-dimethoxypropane to obtain the rosuvastatin calcium key intermediate with a structural formula V. According to the method, tert-butyl bromoacetate and metal organic reagents which are high in cost and difficult to treat are not used, and solvents acetone and acid catalysts are not used in the ketal reaction, so that the production cost is reduced, and the method is more environment-friendly and efficient.

The invention relates to a preparation method of bromoacetic anhydride. The preparation method comprises the following steps: adding a certain amount of organic solvent into a reaction kettle; a certain amount of bromoacetic acid is added, the weight ratio of the organic solvent to the bromoacetic acid is (3-5): 1, a certain amount of acetic anhydride is added, and the ratio of the acetic anhydride to the bromoacetic acid is (1-3): 1; then adding a certain amount of solid acid catalyst resin, wherein the addition amount of the resin is 2-5% of the weight of the bromoacetic acid; the reaction temperature is controlled by the addition of the solvent, and the solvent after reaction can be recycled and reused without loss; due to the addition of the solid acid resin catalyst, the formation of mixed anhydride is effectively inhibited, and the generation of the target product bromoacetic anhydride is promoted; after the reaction is finished, the effective separation of the resin can be realized through precipitation without filtration; the target product can be obtained by distillation after the reaction, so that the operation steps are reduced, and the time is saved; the process is low in raw material cost, simple to operate, high in product quality and easy for industrial production.

The application discloses a preparation process of electronic-grade trans-1,2-cyclohexanediaminetetraacetic acid. The preparation process takes industrial-grade 1,2-cyclohexanediamine as raw material, reacts the 1,2-cyclohexanediamine with electronic-grade organic acid to generate a water-soluble salt, crystallizes at 0-30 DEG C, filters out the crystal to reserve the filtrate, adds an alkaline solution to the filtrate, then adds a polar organic reagent to extract, directly adds an aqueous bromoacetic acid solution to the oil phase to react, after the reaction is completed, adds electronic-grade dilute acid to precipitate trans-1,2-cyclohexanediaminetetraacetic acid until the PH of the system is less than or equal to 2, filters and reserves the solid, washes with pure water, and electronic-grade trans-1,2-cyclohexanediaminetetraacetic acid is obtained. The method has a clear process route, can effectively remove metal ion impurities in the synthesis process, the obtained trans-1,2-cyclohexanediaminetetraacetic acid product has high purity, can be used for preparing high-end semiconductor cleaning liquid, and meets the strict requirements of advanced processes on the purity of cleaning chemicals.

The invention relates to a lead-based perovskite single crystal, a method for controlling growth of the lead-based perovskite single crystal and application of the lead-based perovskite single crystal, and the method for controlling growth of the lead-based perovskite single crystal comprises the following steps: dissolving bromoacetic acid in dimethyl sulfoxide, and heating, stirring and mixing to obtain a mixed solution; adding the mixed solution and a solvent into a mixture of lead chloride, methylamine bromide and lead bromide, and stirring for reaction to obtain a precursor solution; and filtering and heating the precursor solution to obtain the perovskite single crystal. In the crystal growth process, the high-quality perovskite single crystal can be obtained in a short growth period by adjusting nucleation dynamics and maintaining the stability of the growth solution, the contradiction between the growth efficiency of the single crystal and the quality of the single crystal is relieved by utilizing a nucleation inhibition strategy, and on the premise that the sensitivity of a detector is not sacrificed, the high-quality perovskite single crystal can be obtained. The crystal growth period can be effectively shortened.

The invention provides a bromoacetic acid detection method which comprises the following steps: A) reacting a compound, a solvent, alkali and a derivatization reagent to obtain a test solution; reacting bromoacetic acid, a solvent, alkali and a derivatization reagent to obtain a reference solution; b) respectively performing high performance liquid chromatography detection on the test solution and the reference solution to obtain a test chromatogram and a reference chromatogram; and C) calculating the content of bromoacetic acid by an external standard method according to the concentration of the reference substance, the peak area of the reference substance solution in the chromatogram and the peak area of a component, corresponding to the reference substance solution, in the test solution in the chromatogram. The method provided by the invention is good in specificity, good in durability, low in detection limit, low in quantification limit, high in separation degree and relatively accurate in result. The method provided by the invention can be used for accurately detecting each genotoxic impurity in the raw material medicine or the preparation, the separation degree of each peak, the number of theoretical plates and the symmetry factor are good, and the response is high.

The invention discloses a preparation method of a polyoxyethylene / amphoteric polyion liquid type composite solid electrolyte. The preparation method comprises the following steps: S1, reacting bromoacetic acid with 1-vinyl imidazole to obtain carboxylic acid functionalized imidazole chlorine salt; s2, adding lithium salt, washing and drying to obtain carboxylic acid functionalized imidazole trifluoromethanesulfonic acid imine salt; s3, adding a LiOH solution, and reacting to obtain hydroxy acid functionalized ionic liquid; s4, adding a photoinitiator solution to obtain amphoteric polyionic liquid; and S5, adding the polyether diolefin polymer into the polyion liquid, sequentially adding LITFSI, tetrakis (3-thiopropionic acid) pentaerythritol tetrathiol, a thiol chain extender and a photoinitiator, and reacting and drying to obtain the polyoxyethylene / amphoteric polyion liquid type solid electrolyte. According to the obtained solid electrolyte, the lithium ion conductivity is improved, the assembled battery has good electrochemical cycle stability, the service life of the battery is prolonged, and the safety of the battery is improved.

The application discloses a solid-phase extraction membrane based on MOF material and a preparation method and application thereof, and the solid-phase extraction membrane comprises a carrier and an enrichment medium coating loaded on the surface of the carrier; the material of the enrichment medium coating is a defective amino MOF material; the defective amino MOF material is a metal organic framework material prepared by taking zirconium as a metal center, taking dichloroacetic acid as a modulator and reacting with an amino organic ligand; and the carrier is an organic filter membrane. The adsorbent used in the coating of the solid-phase extraction membrane is a defective MOF material prepared by induction of dichloroacetic acid, and the material has the advantages of large adsorption capacity and good chemical stability; the solid-phase membrane coating prepared by taking the material as raw material has the advantages of good water resistance, high enrichment multiple and good reproducibility, and has excellent adsorption effect on bromoacetic acid and iodoacetic acid.

A phenylimidazolium-terminated polyethylene glycol (PEG) corrosion inhibitor and antibacterial water treatment agent and its preparation method are disclosed, comprising the following steps: Step 1: dissolving polyethylene glycol and triethylamine in an anhydrous solvent and cooling the solution to form a reaction system; Step 2: slowly adding bromoacetyl bromide to the reaction system and continuing the reaction to obtain a reaction solution; Step 3: diluting the reaction solution with dichloromethane, removing the triethylamine salt, bromoacetyl bromide, and triethylamine by water extraction, and evaporating after extraction to neutrality to obtain a bromoacetyl-terminated PEG intermediate; Step 4: mixing the intermediate with 1-phenylimidazolium and heating to react to obtain a crude product; Step 5: after the reaction is completed, cooling to room temperature, dialysis in ethanol to purify the product and recover unreacted 1-phenylimidazolium, and evaporating the dialysate to remove ethanol to obtain the phenylimidazolium-terminated PEG corrosion inhibitor and antibacterial water treatment agent. This invention achieves the polymerization, water solubility, and composite functionalization of imidazoline corrosion inhibitors.

The invention discloses a synthesis method of (3-chlorophenethyl) glycine benzyl ester, relates to the technical field of synthesis of (3-chlorophenethyl) glycine benzyl ester, and aims at solving the problems that the yield of (3-chlorophenethyl) glycine benzyl ester is low and production is not easy to amplify. And reacting with benzyl bromoacetate in a reaction solvent to generate (3-chlorophenethyl) glycine benzyl ester. According to the method, sodium carbonate is introduced as a basic catalyst, so that the reaction path is optimized. By accurately regulating and controlling the molar ratio (1: 1.2: 1.2) of 3-chlorophenylethylamine, sodium carbonate and benzyl bromoacetate and adopting the low-temperature (0-10 DEG C) reaction condition, side reaction is effectively inhibited, and the yield of a target product is increased to 85% and is increased by 40% or above compared with that in the prior art; dichloromethane is used as a reaction solvent and has the characteristics of high solubility and low boiling point, and an organic phase can be directly extracted and separated, so that the production period is greatly shortened.

The invention belongs to the field of drug-loaded nano-micelles, and relates to a cystamine-connected carboxymethyl glucan-oleic acid polymer as well as a preparation method and application thereof. The method comprises the following steps: modifying glucan in an alkaline aqueous solution by taking bromoacetic acid as a carboxymethylation reagent to obtain water-soluble carboxymethyl glucan; then coupling the carboxyl of the carboxymethyl glucan with cystamine dihydrochloride, and synthesizing to obtain cystamine-connected carboxymethyl glucan; finally, the carboxyl of oleic acid is coupled with the free amino on the cystamine-connected carboxymethyl glucan, and the cystamine-connected carboxymethyl glucan-oleic acid polymer is obtained. Furthermore, the cystamine-connected carboxymethyl glucan-oleic acid polymer is prepared into a cystamine-connected carboxymethyl glucan-oleic acid polymer blank nano-micelle, and the blank nano-micelle is further loaded with cannabidiol, so that the cannabidiol drug-loaded nano-micelle is obtained. The cannabidiol drug-loaded nano-micelle can enhance accumulation of a tumor site and potentially enhance the tumor treatment effect.

This invention discloses a nickel-cobalt hydrometallurgical recycling process, belonging to the field of hydrometallurgical technology. On one hand, this invention converts magnesium sulfate solution wastewater into magnesium salt solution, replacing sodium hydroxide in saponification with the organic phase, while also saving water in the production line. It also recycles carbon dioxide waste gas, achieving resource conversion and reuse of industrial waste gas. On the other hand, it prepares functional materials to achieve efficient recovery of cobalt and nickel from waste liquid: utilizing Zn... 2+ Coordination activation forms a resin filter membrane with a coordination trap on its surface, which efficiently captures cobalt and nickel ions in waste liquid; a carboxyl-functionalized dimethylglyoxime ligand is pre-synthesized using dimethylglyoxime and bromoacetic acid, and a MOF with a dimethylglyoxime group is directly constructed for chelating Ni. 2+ The prepared adsorption particles undergo secondary adsorption in the waste liquid after passing through the resin, resulting in an extremely high recovery rate of cobalt and nickel ions in the waste liquid. This hydrometallurgical process achieves both recovery and recycling.

The present invention relates to the technical field of trimethylolethane preparation, and specifically discloses a metal-organic framework porous polymer material, a preparation method thereof and an application. The preparation method comprises the following steps: adding a metal chloride into a glutamic acid-halocarboxylic acid ionic liquid, reacting at 100 °C to 140 °C for 2 h to 6 h, adding a sodium alkali salt, and reacting at 70 °C to 110 °C to obtain the metal-organic framework porous polymer material; wherein the halocarboxylic acid is at least one of 3-chloropropionic acid, 4-(chloromethyl)benzoic acid, 3-bromopropionic acid or bromoacetic acid; and the metal chloride is zirconium chloride, iron chloride, zinc chloride or aluminum chloride. The metal-organic framework polymer material prepared by the specific method of the present invention has the advantages of high porosity, many active centers, large specific surface area, is convenient to separate and recover from the system, has good thermal stability, and the catalytic activity does not decrease significantly after being reused multiple times, and has broad application prospects in the field of synthesizing trimethylolethane.

The present invention discloses a ( E The invention relates to a method for preparing a 4-aryl-2,2-difluoro-3-butenoic acid derivative, and belongs to the technical field of pharmaceutical intermediates and organic synthesis. E )-1-aryl-2-bromoethylene and 2,2-difluoro-2-bromoacetic acid derivatives as raw materials, a reductive coupling reaction occurs under the coordinated catalysis of an iron / palladium co-catalyst to generate ( E )-4-aryl-2,2-difluoro-3-butenoic acid derivatives; the synthesized ( E )-4-aryl-2,2-difluoro-3-butenoic acid derivatives contain geminal difluoroallyl structural units and can be used as potential drug candidates. They can also provide a new way to introduce geminal difluoroallyl groups.

The application belongs to the technical field of organic compound synthesis and medicine, and particularly relates to a preparation method of thienopyrimidine mercaptoacetic acid compounds and salts thereof. The method uses an organic base as an acid binding agent, and condenses a mercapto intermediate and 2-bromoacetic acid in an organic solvent to obtain the thienopyrimidine mercaptoacetic acid compound. The compound is reacted with an aqueous base solution in alcohol to form a salt. After the reaction is completed, the solvent is evaporated, acetone is added for pulping, filtration is performed, and drying is performed. The method has mild reaction conditions, simple operation, and high product purity and yield, and is suitable for industrial production.

The invention provides a preparation method of bromoacetic anhydride, and belongs to the technical field of organic synthesis. The invention provides a bromoacetic anhydride preparation method, which comprises: mixing bromoacetic acid and an organic solvent, adding N, N-diisopropyl carbodiimide in batches, and carrying out dehydration condensation to obtain bromoacetic anhydride. According to the method, the dehydrating agent N, N-diisopropylcarbodiimide (DIC) is added in batches, so that water in the system can be consumed by bromoacetic anhydride generated in the early stage, and bromoacetic anhydride generated by reacting the DIC added later with bromoacetic acid in the system is not easy to decompose, so that the raw materials are fully reacted, side reactions are reduced, and the purity and yield of the product are improved.

The utility model relates to the technical field of rectifying kettles, in particular to a rectifying kettle for preparing bromoacetic acid, which comprises an operating table and a kettle body, the kettle body is arranged on the top wall of the operating table and comprises a lower kettle body and an upper kettle body, the bottom wall of the lower kettle body is fixedly connected with the top wall of the operating table, and a hydraulic cylinder I is fixedly arranged on the top wall of the operating table and positioned on the rear side of the kettle body; a connecting frame is fixedly arranged at the output end of the first hydraulic cylinder, the first hydraulic cylinder moves the connecting frame and a connecting arm upwards, the lower kettle body and the upper kettle body can be separated, limiting on the upper kettle body is relieved through a positioning assembly, the upper kettle body can be rotated out from the fixing frame on one side to one side, and therefore the interior of the upper kettle body can be cleaned conveniently; materials for preparing bromoacetic acid can be stirred through the stirring assembly, material residues are reduced, and compared with a traditional rectifying still for preparing bromoacetic acid, the rectifying still with the structure is more convenient to clean.

This invention discloses a magnetic microsphere modified with a high-density carboxyl polymer brush and its preparation method. The method includes the following steps: using ATRP technology, the polymerization of GMA is precisely initiated by an azide-based initiator to synthesize PGMA with controllable molecular weight and narrow distribution; the epoxy groups of PGMA undergo a ring-opening reaction with ethylenediamine, followed by reaction with bromoacetic acid to obtain a functionalized polymer brush; utilizing the high efficiency and specificity of azide-alkynyl click chemistry, the carboxylated polymer brush is covalently grafted onto the surface of the magnetic microspheres. This invention achieves precise design of the polymer brush molecular structure and successfully prepares magnetic microspheres with significantly increased carboxyl content, up to a maximum content of 1.495 mmol·g. ‑1 The polymer brush modification strategy of this invention significantly improves the functional group density on the surface of microspheres and their binding ability with biomolecules. The resulting magnetic microspheres have strong magnetic responsiveness and are not easily leaked. They can be used as high-performance platform materials and are widely used in fields such as bioseparation, diagnostic analysis and catalysis.

The invention relates to the technical field of wastewater treatment, and in particular to an MS-MIL-53-PAN material for removing cobalt ions from wastewater and a preparation method thereof. The material is prepared from the following raw materials: molecular sieve MS, aminopropyltrimethoxysilane APS, bromoacetic acid, terephthalic acid and polyacrylonitrile PAN. The preparation method comprises the following steps: reacting the molecular sieve MS, aminopropyltrimethoxysilane APS and bromoacetic acid to obtain a carboxylated molecular sieve MS-COOH; reacting the carboxylated molecular sieve MS-COOH with terephthalic acid; and preparing the MS-MIL-53-PAN material for removing cobalt ions from wastewater by electrostatic spinning. The prepared MS-MIL-53-PAN material for removing cobalt ions from wastewater can be effectively used to treat cobalt ion radioactive wastewater, thereby reducing the threat to human health and environmental safety.

The preparation method specifically comprises the following steps: firstly, synthesizing an intermediate N, N-dimethyl heptadecyl amido ethylenediamine, then mixing bromoacetic acid, water and absolute ethyl alcohol, carrying out heating and stirring reaction, slowly dropwise adding N, N-dimethyl heptadecyl amido ethylenediamine after bromoacetic acid is completely dissolved, carrying out heating and stirring reaction for 2-3 hours, and then, carrying out heat preservation for 2-3 hours, so as to obtain the temperature-sensitive self-defoaming foam scrubbing agent. And carrying out reduced pressure distillation to remove the solvent ethanol and water, washing, filtering, and drying to obtain the temperature-sensitive self-defoaming bubble scrubbing agent. The temperature-sensitive self-defoaming foam scrubbing agent disclosed by the invention not only has relatively good foaming performance and stability, but also has temperature-sensitive performance and self-defoaming capability, and phase transformation can be carried out according to the change of the environment temperature of a gas well shaft in a foam scrubbing process, so that foaming components are separated out to realize defoaming; and moreover, the investment of a defoaming agent can be reduced, even the defoaming agent is not needed, a new technical thought is provided for drainage gas recovery of an oil and gas field, and the method has important mine field application value.

The present application relates to a method for detecting bromoacetic acid as an impurity in cefathiamidine. The detection method adopts high performance liquid chromatography-mass spectrometry, wherein the conditions of high performance liquid chromatography are: mobile phase A: water; mobile phase B: acetonitrile; wherein mobile phase A and mobile phase B are used for gradient elution. The method of the present application has a low detection limit of bromoacetic acid in cefathiamidine and high sensitivity, and can efficiently detect and control bromoacetic acid in cefathiamidine at the ng / ml level, which is of great significance to the quality control and pharmaceutical safety of cefathiamidine.

The invention provides a preparation method of a zavazepam intermediate 3-(piperidine-4-yl)-1, 2-dihydroquinoline-2-ketone or a salt of the zavazepam intermediate 3-(piperidine-4-yl)-1, 2-dihydroquinoline-2-ketone. The preparation method comprises the following steps: by taking tert-butyl bromoacetate and trimethyl orthoformate as raw materials, carrying out condensation to obtain 2-bromoalkene tert-butyl propionate, then carrying out Suzuki coupling on the 2-bromoalkene tert-butyl propionate and N-tert-butyloxycarboryl piperidine-4-boronic acid pinacol ester to obtain 2-(N-tert-butyloxycarboryl piperidine-4-yl) tert-butyl acrylate, and then hydrolyzing the 2-(N-tert-butyloxycarboryl piperidine-4-yl) tert-butyl acrylate to obtain an acrylic acid derivative. The preparation method comprises the following steps: directly constructing a quinoline-2-ketone core skeleton by coupling-cyclizing acrylic acid and 2-bromoaniline through a one-pot method in the presence of palladium catalysis and a dehydrating agent to obtain a Boc protection intermediate, and finally performing acidolysis deprotection to obtain a target product. The route thoroughly avoids sodium hydride, LDA, iron powder and other dangerous or high-pollution reagents, conditions are mild, operation is safe, three wastes are few, all intermediates and products can be purified through conventional crystallization, column chromatography is not needed, the total yield is high, and the method is suitable for industrial production.

The invention provides an isoindolone-containing CDK4 / 6 inhibitor and a preparation method and application thereof.The preparation method comprises the steps that ethyl bromoacetate is introduced to a piperazine group of a palbociclib structure to be hydrolyzed into acid, then amido bonds are generated to be linked with different isoindolone, and a series of compounds shown in the formula I are synthesized; the compound can be used for preventing or treating mammalian diseases related to abnormal expression of CDK4 / 6 and anti-tumor, anti-virus, antibacterial and anti-inflammatory related to CDK4 / 6. I.

The invention discloses an electrocatalyst as well as a preparation method and application thereof, and belongs to the technical field of hydrogen production by electrocatalytic decomposition of water. The electrocatalyst is a nickel-iron alloy / nickel iron oxide / carboxymethyl polyaniline / foam iron (NiFe-O at c-PANI / IF); the microstructure of the electrocatalyst is in a nanosheet shape. The preparation method of the electrocatalyst comprises the following steps: firstly, dissolving nickel acetate, ammonium sulfate and aniline in water, carrying out electrodeposition reaction for 30 minutes, and drying; adding a bromoacetic acid solution and soaking for 6 hours; and the composite material NiFe-O at c-PANI / IF is obtained. The composite material is used as an electrocatalyst for catalyzing OER reaction, and is high in reaction activity and good in stability. The prepared NiFe-O (at) c-PANI / IF serves as an anode and a cathode at the same time, an electrolytic tank (NiFe-O (at) c-PANI / IFNiFe-O (at) c-PANI / IF) is formed and used for electrolyzing water, and a good catalytic effect is achieved; and meanwhile, the catalytic stability of the electrolyzed water of the electrolytic tank is good, and the performance of the electrolyzed water is not obviously reduced after 1100 h i-t test.

The invention provides a method for detecting genotoxic impurity methyl bromoacetate in a compound 2-((5-bromo-4-(2-chloro-4-cyclopropylnaphthyl-1-yl)-4H-1, 2, 4-triazole-3-yl)-sulfur) acetic acid, which comprises the following steps: reacting the compound, a solvent, triethylamine and a derivatization reagent to obtain a test solution; the compound is-((5-bromo-4-(2-chloro-4-cyclopropyl naphthyl-1-yl)-4H-1, 2, 4-triazole-3-yl)-sulfur) acetic acid, and the structural formula of the compound is shown in the description. Methyl bromoacetate, a solvent, triethylamine and a derivatization reagent are subjected to a reaction, and a reference substance solution is obtained; and respectively performing high performance liquid chromatography detection on the test solution and the reference solution to obtain a test chromatogram and a reference chromatogram. The method provided by the invention is good in specificity and good in durability. The method provided by the invention can be used for accurately detecting each genotoxic impurity in the raw material medicine or the preparation, the separation degree of each peak, the number of theoretical plates and the symmetry factor are good, and the response is high.

The embodiment of the invention provides a porous material and application thereof, and relates to the technical field of electronic gas. The porous material is applied to adsorption of electronic special gas. The porous material is a metal organic framework material and is formed by a metal oxygen cluster, a tricarboxylic acid organic ligand and a halogenated acetic acid ligand. Wherein the halogenated acetic acid ligand is selected from one or more of difluoroacetic acid, dichloroacetic acid, dibromoacetic acid and diiodoacetic acid. The metal organic framework material can adsorb electronic special gas, has high pore volume and high specific surface area, and can improve the desorption rate and delivery amount of the electronic special gas.