18 results about "Bromoacetic acid" patented technology

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 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 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 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 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.

This invention discloses a synthetic method for preparing tert-butyl bromoacetate using a combination of microchannel and molecular distillation, belonging to the field of chemical technology. The invention involves feeding bromoacetic acid and isobutylene into a microchannel reactor via a metering pump, controlling parameters such as the feed molar ratio, mass flow rate, residence time, reaction temperature, and pressure. The reaction solution is then fed into a molecular distillation apparatus to separate the product, controlling the feed rate and distillation temperature. Unreacted isobutylene is recovered and returned to the reaction system for recycling. The synthetic apparatus includes modules for feeding, reaction, separation and purification, product collection, and temperature control. This method features fast reaction speed, low energy consumption, high product yield, selectivity, and purity, ensuring reaction consistency and economic efficiency, achieving raw material recycling and green production. The synergistic effect of the microchannel reactor and molecular distillation, combined with precise control and a closed-loop reaction, offers significant advantages.

The invention discloses a synthesis method of a benzofuro [3, 2-b] benzofuran compound, and belongs to the technical field of organic synthesis. According to the method, o-hydroxybenzoate compounds or halogenated derivatives thereof and methyl bromoacetate are taken as starting raw materials, and a target product is prepared through five steps of reaction: step 1, cyclization is performed at 0 DEG C to room temperature under an alkaline condition to obtain a benzofuran carboxylate intermediate; 2, sulfonylating by trifluoromethanesulfonic anhydride to obtain a sulfonate intermediate; 3, carrying out an etherification reaction with an o-halogenated phenol compound at the temperature of 80-120 DEG C; 4, hydrolyzing through inorganic strong base to obtain a benzofuran carboxylic acid intermediate; and 5, carrying out intramolecular ring closing at 80-180 DEG C under the action of a palladium catalyst and DBU. The raw materials are cheap and easy to obtain, the reaction selectivity is high, the total yield is stable, the substrate adaptability is wide, efficient synthesis of unilateral and bilateral halogen substituted derivatives of benzofuro [3, 2b] benzofuran compounds is successfully achieved, and the method has remarkable industrial application value.

The application provides a synthesis method of metrafenone, and belongs to the technical field of organic synthesis, and comprises the following steps: firstly, subjecting 5-hydroxy-1-methyl-3-(trifluoromethyl)-1H-pyrazole to a hydroxymethylation reaction to obtain 4-(hydroxymethyl)-5-hydroxy-1-methyl-3-(trifluoromethyl)-1H-pyrazole; then, reacting with difluorobromoacetic acid to obtain 4-(hydroxymethyl)-5-(difluoromethoxy)-1-methyl-3-(trifluoromethyl)-1H-pyrazole; then, subjecting to a mesylation reaction to obtain a mesylate intermediate; simultaneously, preparing 3-acetylthio-5,5-dimethyl-4,5-dihydroisoxazole from 3-chloro-5,5-dimethyl-4,5-dihydroisoxazole; then, subjecting the intermediate to a thioetherization reaction with the mesylate intermediate to obtain a thioether coupling intermediate; finally, performing an oxidation reaction in the presence of a catalyst to obtain metrafenone. By adopting the mesylate activated intermediate and combining a continuous flow fixed bed oxidation process, the method is favorable for improving the purity and total yield of the target product and reducing the tungsten residue in the product.

The invention discloses a preparation method of an antiviral drug amonevir. The method comprises the following steps: pumping sulfurized cyclopentane-4-formyl chloride prepared in situ and 2, 6-dimethylaniline into a first microchannel reactor, and carrying out an amidation reaction; pumping the obtained amide intermediate, potassium tert-butoxide and bromoacetic acid into a second microchannel reactor, and carrying out a second amidation reaction; pumping the generated product, 4-(1, 2, 4-oxadiazole-3-yl) aniline and a condensing agent into a third microchannel reactor, and carrying out a third amidation reaction; pumping the obtained product and hydrogen peroxide into a fourth micro-channel reactor for oxidation reaction to obtain an amonevir crude product; and after the crude product is subjected to extraction, concentration and ethanol recrystallization, an amonevir product with liquid phase purity of 99.9% is obtained. And the tautomer of the amonevir can be simply and efficiently separated by utilizing the detection method disclosed by the invention, and a reliable guarantee is provided for industrial production of the amonevir.

The invention discloses a preparation method of an alkynyl bicyclo [3.1. 1] heptane difluoroacetate compound in the technical field of organic synthesis, which comprises the following steps: by taking terminal alkyne, [3.1. 1] propeller alkane and gem-difluorobromoacetate as initial raw materials, under the condition that the stoichiometric copper acetylacetonate and 1, 8-diazabicyclo [5.4. 0] undec-7-ene (DBU) are taken as alkalis and acetonitrile is taken as a solvent, carrying out a reaction on the initial raw materials to prepare the alkynyl bicyclo [3.1. 1] heptane difluoroacetate compound. The reaction is carried out through a one-pot method. The process comprises the following key steps: firstly, generating high-activity gem-difluoroacetate free radicals from gem-difluorobromoacetate; the free radical and high-tension [3.1. 1] propeller alkane are subjected to ring-opening addition, ring tension is released, and a new carbon center free radical intermediate is generated; the intermediate is then captured by alkynyl copper species generated in situ, and finally a target product is obtained through reduction elimination. The method is mild in reaction condition and wide in substrate universality, the problems of tedious synthesis steps and low efficiency in the prior art are solved, and a novel and efficient way is provided for preparation of the important molecules.

The invention discloses a preparation method of a gadotetrol isomer. The method comprises the following steps: by taking cycleanine as an initial raw material, firstly reacting with tert-butyl bromoacetate to obtain a trisubstituted intermediate; then in the presence of a reducing agent, carrying out reductive amination reaction with hydroxyacetone, and directionally introducing a 1-hydroxy-propyl-2-yl side chain; and removing a protecting group through alkaline hydrolysis, carrying out chelation reaction with a gadolinium source, and purifying to obtain the gadotetrol isomer. The method adopts a reductive amination strategy to solve the problem of regioselectivity, is combined with an alkaline hydrolysis process, has the advantages of short synthesis route, high total yield, mild reaction conditions, simplicity and convenience in operation and the like, effectively avoids the use of high-pressure hydrogenation and highly toxic reagents, and is suitable for industrial preparation.

The invention discloses a polyaspartic acid-based quaternary ammonium salt for scale and corrosion inhibition and a preparation method and application thereof, and belongs to the technical field of industrial circulating water treatment.The preparation method comprises the steps that N, N-dimethylethylenediamine is introduced into a peptide chain of polyaspartic acid through a graft copolymerization method, then quaternary ammonium salinization is conducted on an intermediate through bromoacetic acid, and the polyaspartic acid-based quaternary ammonium salt is obtained; a target compound, namely polyaspartic acid-based quaternary ammonium salt is synthesized, the compound can be combined with metal ions such as Ca < 2 + > to generate a water-soluble complex, and the compound has certain scale and corrosion inhibition performance. Therefore, the scale and corrosion inhibition performance of the polyaspartic acid-based quaternary ammonium salt is remarkably improved, meanwhile, application of phosphorus-containing compounds is avoided, and the negative influence on the environment is effectively relieved.