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171 results about "Bromobenzenes" patented technology

Derivatives of benzene in which one or more hydrogen atoms on the benzene ring are replaced by bromine atoms.

Crown ether functionalized covalent organic framework material as well as preparation method and application thereof

The invention discloses a crown ether functionalized covalent organic framework material as well as a preparation method and application thereof, and the method comprises the following steps: adding a covalent organic framework material, 4-bromobenzo-15-crown-5, potassium carbonate and potassium iodide into an acetone solution for reaction, washing the obtained crude product, performing Soxhlet extraction with tetrahydrofuran for a certain time, and drying to obtain the crown ether functionalized covalent organic framework material. The crown ether functionalized covalent organic framework material is obtained. Compared with a synthesis method of crown ether functionalized COFs in the prior art, the method has the advantages that the crown ether (4-bromobenzo-15-crown-5) can be grafted to the COFs in one step, the Na < + > adsorption capacity and the adsorbent recycling performance are greatly improved, the synthesis method is simple, and synthesis of the crown ether functionalized COFs is greener, more convenient and more economical.
Owner:QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI

Synthesis process of 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride

PendingCN121021334AHydrazine preparationOrganic-compounds/hydrides/coordination-complexes catalystsPhenylhydrazine hydrochlorideIodide
The invention relates to the technical field of chemistry, in particular to a synthesis process of 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride, which comprises the following steps: by taking 4-fluoro-3, 5-dimethylbromobenzene as a raw material and hydrazine hydrate as a hydrazine source, matching with alkali such as potassium hydroxide, sodium hydroxide or potassium phosphate and the like, reacting at the temperature of 60-80 DEG C to obtain the 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride. The preparation method comprises the following steps: by taking copper or nickel source catalysts such as cuprous bromide, cuprous iodide, nickel salicylate and the like, N, N-bis (2, 6-dimethylphenyl) oxamide as a ligand, hexadecyl trimethyl ammonium bromide as a stabilizer and a dioxane-water mixed system as a solvent, reacting at 80-110 DEG C under the protection of nitrogen, separating a reaction mixed solution after the reaction is finished, and separating the reaction liquid to obtain the target product. And purifying to obtain a finished product of the 4-fluoro-3, 5-dimethyl phenylhydrazine hydrochloride. Therefore, the problems that the synthesis of the 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride is poor in safety, low in production efficiency, poor in environmental friendliness, small in substrate application range and the like are solved.
Owner:NANJING QINUO PHARMACEUTICAL TECHNOLOGY CO LTD +1

Method for synthesizing platinum-based nitrogen-doped graphdiyne catalyst based on atomic layer deposition technology and application thereof

The invention discloses a method for synthesizing a platinum-based nitrogen-doped graphdiyne catalyst based on an atomic layer deposition technology and application of the platinum-based nitrogen-doped graphdiyne catalyst. Firstly, hexabromobenzene and calcium carbide are subjected to vacuum ball milling, calcination and purification to obtain a graphdiyne carrier, then the graphdiyne carrier and melamine are mixed and calcined to achieve nitrogen doping of the carrier, and then loading of platinum nanoparticles is accurately controlled through an atomic layer deposition technology. According to the method, the characteristics of an atomic layer deposition technology are utilized, deposition parameters and the number of cycles are controlled, uniform distribution and size control of Pt nano-particles on porous graphdiyne are achieved, and a nitrogen-doped graphdiyne carrier and the platinum nano-particles have a synergistic effect. The platinum-based nitrogen-doped graphdiyne catalyst prepared by the invention has the specific surface area of 734.8 m < 2 > g < 1 > and the average pore size of 8.68 nm, and shows excellent electrocatalytic activity and dynamic performance in reaction.
Owner:HENAN NORMAL UNIV

Chloromethylation catalyst, preparation method and method for preparing high-purity ortho-position, meta-position and para-position chloromethyl styrene by using chloromethylation catalyst

The invention relates to the technical field of catalytic synthesis, in particular to a chloromethylation catalyst, a preparation method of the chloromethylation catalyst and a method for preparing high-purity ortho-position, meta-position and para-position chloromethyl styrene through the chloromethylation catalyst, and the chloromethylation catalyst is prepared by loading sulfonic acid compounds and (or) pyridine compounds and (or) copper salt on a molecular sieve. The method can improve the localization selectivity of chloromethylation. The method for preparing high-purity ortho-position, meta-position and para-position chloromethyl styrene comprises the following steps of: reacting beta-bromophenylethane, paraformaldehyde and lewis acid in the presence of the chloromethylation catalyst to generate chloromethyl beta-bromophenylethane, and then performing elimination reaction under an alkaline condition to generate a chloromethyl styrene crude product; the high-purity ortho-position, meta-position and para-position chloromethyl styrene is obtained after the crude product is rectified, the brand-new catalyst is adopted in the method, the reaction selectivity is enhanced, the process is simple, and industrial production is facilitated.
Owner:NANJING MAIN LIFE TECH CO LTD

A method for analyzing benzothiazole-based contaminants

This invention discloses an analytical method for benzothiazole contaminants, comprising the following steps: detection by high performance liquid chromatography (HPLC), with the following chromatographic conditions: a phenylhexyl column as the stationary phase, mobile phase A being water, mobile phase B being acetonitrile, and gradient elution; wherein the benzothiazole contaminants are at least one of 2-aminobenzothiazole, 2-hydroxybenzothiazole, benzothiazole, 2-methylbenzothiazole, 2-mercaptobenzothiazole, 2,5-dimethylbenzothiazole, 2-cyanobenzothiazole, ethyl 2-carboxylate benzothiazole, 2-chlorobenzothiazole, 2-bromobenzothiazole, 2-methylthiobenzothiazole, phenylthiocyanate, N-tert-butyl-2-benzothiazole sulfenamide, 2-(2-hydroxyphenyl)-benzothiazole, N-cyclohexyl-2-benzothiazole sulfinamide, dibenzothiazole disulfide, and N,N-dicyclohexyl-2-benzothiazole sulfonamide.
Owner:CHUZHOU VOCATIONAL & TECHN COLLEGE

Preparation method of pinoxaden

The invention relates to a pinoxaden preparation method, which comprises: S1, carrying out a cyclization reaction on hydrazine hydrate and a compound represented by a formula (I) to generate an intermediate 1; s2, reacting the intermediate 1 with a compound as shown in a formula (II) in the presence of alkali to generate an intermediate 2; s3, enabling the intermediate 2 to react with 2, 6-diethyl-4-methyl bromobenzene under the action of a catalyst to generate an intermediate 3; s4, the intermediate 3 and pivaloyl chloride react in the presence of alkali, pinoxaden is obtained, the structural formula of the intermediate 1 shown in the formula (I) is shown in the description, the structural formula of the intermediate 2 shown in the formula (II) is shown in the description, and the structural formula of the intermediate 3 shown in the description is shown in the description.
Owner:JIANGSU SEVENCONTINENT GREEN TECH RES INST CO LTD +1

Indole allylamine amide derivative as well as preparation method and application thereof

The invention belongs to the field of medicinal chemistry, and relates to an indole allylamine amide derivative as well as a preparation method and application thereof. Functional activity screening of G protein dependent signaling pathways is carried out on all the synthesized compounds, and it is found that the new derivatives can be used for preparing beta2-adrenergic receptor allosteric antagonism regulator drugs. Trans-indole allylamine is used as a raw material, amide coupling is performed to obtain the novel indole allylamine amide derivative, and R1 is any one of phenyl, m-methylbenzene, m-methoxyphenyl, m-bromophenyl, m-chlorphenyl, m-fluorophenyl, o-methoxyphenyl, p-methoxyphenyl, naphthalene ring, oxazole, cyclohexyl, cyclopentyl, methyl, ethyl and isopropyl. A biological activity test result shows that the indole allylamine amide derivative disclosed by the invention has relatively good antagonistic activity on beta2AR and can be used for carrying out negative allosteric regulation on the functional activity of isoproterenol.
Owner:CHANGZHOU UNIV

Preparation method of 3-substituted isocoumarin compound

The invention discloses a preparation method of a 3-substituted isocoumarin compound, and belongs to the technical field of coumarin compound synthesizing.The preparation method comprises the steps that a 2-bromophenylboronic acid compound and alkyne serve as reaction substrates, a bidentate nitrogen ligand is added and dissolved in a solvent, under the action of alkali and a copper catalyst, a normal-pressure one-step cyclization reaction is conducted in the CO2 atmosphere, and the 3-substituted isocoumarin compound is obtained. The 3-substituted isocoumarin compound is obtained. According to the method, CO2, alkyne and 2-bromophenylboronic acid are used as reaction raw materials, cheap copper is used as a catalyst, the use amount is small, the 3-substituted isocoumarin is obtained through carbon-carbon coupling-cyclization by a CO2 activation one-step method under normal pressure, the conditions are mild, the cost is low, and the method is environmentally friendly.
Owner:CHENGDU UNIVERSITY OF TECHNOLOGY

Preparation and application of covalent organic framework photocatalyst for photocatalytic CO2 reduction

The invention discloses a preparation method of a covalent organic framework photocatalyst for photocatalytic reduction of CO2, which comprises the following steps: adding 4, 4 ', 4' '-(1, 3, 5-triazine-2, 4, 6-triyl) triphenylamine and 2, 5-dibromobenzene-1, 2, 4, 5-tetracarboxylic dianhydride into a reaction kettle, then adding 1-hydroxy-3-methylbenzene and isoquinoline, and uniformly mixing; and carrying out microwave heating on the reaction kettle, cooling to room temperature, filtering, collecting precipitate, washing, and then carrying out Soxhlet extraction and vacuum drying to obtain the covalent organic framework photocatalyst. A surface halogen atom modification strategy is designed and used for regulating and controlling electron distribution and light capture capacity of a donor-acceptor (D-A) in TzPm-COF, and results show that the strategy can effectively improve photocatalytic activity and selectivity of reduction of CO2 into CO, and can be applied to preparation of the TzPm-COF catalyst. A reasonable design strategy is provided for developing a functional modified COFs material for efficiently and selectively photocatalytic CO2 reduction.
Owner:SOUTHWEAT UNIV OF SCI & TECH

(E)-1, 4-diether olefin and preparation method thereof

The invention discloses (E)-1, 4-diether olefin and a preparation method thereof, and the (E)-1, 4-diether olefin is obtained by using 1, 3-diene as a raw material and carrying out electrochemical reaction in the presence of an electrolyte and a solvent, wherein the 1, 2, 4-trimethyl-1, 3- The structural formula of the 1, 3-diene is as follows: R1 is phenyl, p-fluorophenyl, p-chlorphenyl, p-bromophenyl, p-methylphenyl, p-methoxyphenyl, p-trifluoromethylphenyl, p-trifluoromethoxyphenyl, p-acetoxyphenyl, p-methyl formate phenyl, p-cyanophenyl, p-pinacol borate phenyl, p-phenylphenyl, o-oxybenzyl phenyl and o-methoxyphenyl; r1 is one of 1, 2-naphthyl; the solvent is a mixed solvent containing methanol. The preparation method of (E)-1, 4-diether olefin has high E-selectivity and 1, 4-selectivity, and an electro-catalysis mode is adopted, so that the use of a stoichiometric toxic, expensive or dangerous oxidant is avoided.
Owner:HEFEI UNIV OF TECH

A method for preparing 2-aminopyridopyrimidinones

ActiveCN122356051BOrganic synthesisOrganosolv
The application provides a preparation method of 2-aminopyridopyrimidinone compounds, which comprises the following steps: reacting 2-bromo-N-phenyl nicotinamide compounds and monocyanoamine in an organic solvent in the presence of alkali to obtain 2-aminopyridopyrimidinone compounds. The method has the advantages of no metal catalysis, mild reaction conditions, high atom economy, wide substrate applicability and simple operation, and has important application value in the fields of medicinal chemistry and organic synthesis.
Owner:NINGXIA UNIVERSITY

Synthesis method of deuterated m-dibromobenzene-D4

The invention belongs to the technical field of deuterated organic chemical synthesis, and particularly relates to a synthetic method of deuterated m-dibromobenzene-D4, which comprises the following steps: a, nitration reaction of deuterated benzene: enabling the deuterated benzene to react with mixed acid to generate deuterated nitrobenzene; b, performing bromination reaction on the deuterated nitrobenzene: reacting the deuterated nitrobenzene with liquid bromine by taking iron tribromide as a catalyst to generate deuterated m-bromo nitrobenzene; c, carrying out reduction reaction on the deuterated m-bromonitrobenzene: converting the deuterated m-bromonitrobenzene into deuterated m-bromoaniline by taking biboric acid as a reducing agent; and d, diazotization reaction of the deuterated m-bromoaniline: enabling the deuterated m-bromoaniline to react with cuprous bromide to generate the target product deuterated m-dibromobenzene. The deuterated m-dibromobenzene-D4 product with high purity and deuterated rate is prepared by the synthetic method, the process is simple, the raw materials are low in price and easy to obtain, and the application of the deuterated halogenated aromatic hydrocarbon serving as an intermediate in synthesis in the fields of organic photoelectricity and deuterated medicines is expanded.
Owner:PERRY TECH CO LTD

Efficient synthesis method of brexpiprazole

The invention discloses an efficient synthesis method of brexpiprazole, which comprises the following steps: taking 4-bromo-benzothiophene and N-Boc-piperazine as initial raw materials, under the protection of nitrogen, carrying out reaction by using a supported catalyst to prepare 4-Boc piperazine benzothiophene, and then carrying out acidolysis to obtain 4-piperazine benzothiophene hydrochloride; the method comprises the following steps: reacting 3, 4-dihydro-7-hydroxy-2 (1H) quinolinone with 1-bromo-4-chloro-butane to generate 3, 4-dihydro-7-(4-chlorobutoxy)-2 (1H)-quinolinone, and then converting the 3, 4-dihydro-7-(4-chlorobutoxy)-2 (1H)-quinolinone into 7-(4-chlorobutoxy)-2 (1H)-quinolinone; then condensing with 4-piperazine benzothiophene hydrochloride to obtain a crude product of brexpiprazole; and finally, crystallizing and purifying for multiple times to obtain high-purity brexpiprazole. According to the preparation method disclosed by the invention, 4-bromo-benzothiophene and N-Boc-piperazine are taken as starting raw materials, and high-purity brexpiprazole is prepared by optimizing selection of a catalyst and conditions of each step and through an excellent purification process.
Owner:SUZHOU JINGYE MEDICINE & CHEM

Process for the preparation of o-bromoanisole

The application discloses a preparation method of o-bromoanisole. The o-bromoanisole is synthesized through three steps, anisole is used as raw material, p-sulfonic anisole is first synthesized, 2-bromo-4-sulfonic anisole is synthesized on the basis, and finally, the sulfonic group is removed to obtain o-bromoanisole. Since anisole is used as raw material, the problems of multiple by-products, low yield and low purity existing in the synthesis path of phenol are avoided. Meanwhile, all the raw materials of the application have low cost, the process steps are simple, and etherification is not needed. Meanwhile, since anisole is used as raw material, hydrobromic acid and hydrogen peroxide can be used in the intermediate step, the hydrobromic acid is oxidized to generate bromine, the reaction rate can be controlled, the reaction efficiency is improved, the waste of bromine is reduced, the purity of the prepared product can reach 99.4%, the yield reaches 96.26%, and the product can be applied on a large scale in industry.
Owner:SANMENXIA AOKE TECH CO LTD

Preparation method of 4-chloromethylstyrene

The invention discloses a preparation method of 4-chloromethylstyrene, and belongs to the technical field of synthesis of organic intermediates. 4-bromobenzaldehyde is adopted as a raw material and reacts with ethylene glycol under the action of p-toluenesulfonic acid to generate an intermediate 1; reacting with magnesium metal to generate a Grignard reagent, reacting with acetaldehyde, and hydrolyzing to generate an intermediate 2; finally, under the combined action of methyl dichlorosilane and tri (pentafluorophenyl) boron, the product 4-chloromethyl styrene is generated. The raw materials can be obtained in the market, the reaction of dehydrating benzyl alcohol into olefin and directly chlorinating aldehyde group to generate benzyl chloride is completed by a one-step method under the combined action of methyl dichlorosilane and tris (pentafluorophenyl) boron, the operation is simple and convenient, the overall yield is high, and a route reference is provided for synthesizing the compounds.
Owner:安徽英特美科技有限公司

Synthesis method of bis-ethyl hexyloxyphenol methoxyphenyl triazine

The invention discloses a synthesis method of bis-ethyl hexyloxyphenol methoxyphenyl triazine, which relates to the technical field of organic chemistry, and comprises the following steps: preparing an intermediate I, putting zinc chloride into reaction, adding xylene for dispersion, dropwise adding the intermediate I, resorcinol and xylene solvent to obtain a yellow intermediate II crude product, and then adding the yellow intermediate II crude product into the reaction kettle to obtain the bis-ethyl hexyloxyphenol methoxyphenyl triazine. Adding the intermediate II, a xylene solvent, an acid-binding agent, chloro-isooctane and bromo-isooctane into a reaction kettle, carrying out reaction treatment to obtain a high-purity product, and carrying out sampling detection on the step 1, the step 2 and the step 3. According to the synthesis method of the bis-ethyl hexyloxyphenol methoxyphenyl triazine, p-bromoanisole and chloro-isooctane or bromo-isooctane are adopted as raw materials, the production cost is reduced, xylene is a single solvent, the problem that a mixed solvent is difficult to recycle is solved, anhydrous aluminum chloride or anhydrous zinc chloride is adopted as a catalyst, and a recrystallization technology is adopted, so that the yield of the bis-ethyl hexyloxyphenol methoxyphenyl triazine is increased. The purity of the product is improved, and the bis-ethyl hexyloxyphenol methoxyphenyl triazine with higher purity is prepared.
Owner:SANMENXIA AOKE TECH CO LTD

A method for synthesizing a tenapano hydrochloride intermediate

PendingCN122301770APtru catalystEnamine
This invention discloses a method for synthesizing a tenapano hydrochloride intermediate. The synthesis method includes the following steps: (1) condensing the compound 3-bromophenylacetaldehyde and the compound N-methyl-(2,4-dichlorophenyl)methylamine under dehydration conditions to obtain an enamine intermediate; (2) subjecting the enamine intermediate to an intramolecular cyclization reaction in the presence of an acid catalyst to obtain the tenapano hydrochloride intermediate 4-(3-bromophenyl)-6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinoline. The synthetic route provided by this invention requires only two steps to construct the key framework, and has the advantages of short reaction steps, high overall yield, and no need to use highly toxic liquid bromine. This process has high atom economy, reduces the emission of waste gas, wastewater, and solid waste, and is suitable for large-scale industrial production under mild conditions.
Owner:JIANGSU HAIYUEKANG PHARM TECH CO LTD

Improved ionogel confined palladium on carbon catalyst, its preparation method and application

PendingCN122273579APalladium on carbonPhosphorous acid
This invention relates to the field of fine chemical catalysis technology, specifically to an improved ion-gel confined palladium-on-carbon catalyst, its preparation method, and its applications. The catalyst uses N,N-dimethylacetamide (DMAc) as a solvent and potassium acetate as a base, with the addition of a catalytic amount of antioxidant 168 [(tris(2,4-di-tert-butylphenyl) phosphite)], and the reaction is carried out under milder CO pressure (1.0-1.6 MPa) and temperature (90-110 °C). This improved catalyst, in synergy with the optimized process, unexpectedly enables the high conversion and selectivity of 4-bromobenzyl sulfone derivatives to 4-methylsulfonylbenzoic acid derivatives, while maintaining the catalyst's excellent recyclability and stability. This invention provides a highly efficient, green, and easily industrialized synthetic route for the target product.
Owner:YULIN UNIV

Bromine flame retardant containing secondary amine reaction sites for epoxy resin and preparation method of bromine flame retardant

The invention provides a bromine flame retardant containing secondary amine reaction sites for epoxy resin and a preparation method of the bromine flame retardant. The preparation method of the flame retardant comprises the following steps: dissolving tetrabromophthalic anhydride, adding primary amine containing a secondary amine group for reaction, and removing a solvent to obtain the bromine flame retardant containing the secondary amine, a carboxylic acid group and a bromine element at the same time. The flame retardant is liquid at room temperature and is convenient to use, and meanwhile, the molecular structure of the flame retardant contains secondary amine, carboxylic acid groups and bromine elements, so that the flame retardant can participate in an epoxy reaction, and meanwhile, a promoting effect and excellent product flame retardant performance are provided for an amine reaction.
Owner:WANHUA CHEM GRP CO LTD

Synthesis method of high-purity benzocyclobutenyl organosilicon monomer for semiconductor packaging resin

The invention discloses a synthesis method of a high-purity benzocyclobutenyl organosilicone monomer for semiconductor packaging resin, which specifically comprises the following steps: by taking vinyl silane and 4-bromobenzocyclobutene as reaction raw materials, firstly preparing benzocyclobutene-vinyl silane through Heck reaction, and then preparing benzocyclobutene-vinyl silane by taking a Meerwein reagent as a medium and potassium carbonate as an additive, thereby obtaining the high-purity benzocyclobutenyl organosilicone monomer for semiconductor packaging resin. And carrying out mild reaction in a polar aprotic solvent to directly prepare the high-purity benzocyclobutene organic silicon monomer tetramethyl divinyl siloxane dibenzocyclobutene. Compared with the traditional preparation method, the method has the advantages of wide reaction raw material source, low price, few reaction steps and high yield in synthesis, and the reaction is beneficial to the high purification process of the monomer, so that the method is more suitable for industrial batch production.
Owner:SOUTHWEAT UNIV OF SCI & TECH

A polyurethane automotive topcoat and a method of making the same

The application discloses a polyurethane automobile finish and a preparation method thereof, and relates to the field of automobile finishes. In the preparation of the polyurethane automobile finish, titanium white powder, 3-buten-1, 2-diol and 6-bromo-3-(4-bromophenyl)-2, 4-dihydro-1, 3-benzoxazine are uniformly mixed to prepare modified titanium white powder; microcrystalline cellulose is aldehyde-based after being grafted with n-butyric acid, acetic anhydride and 2-aminopiperazine to obtain modified cellulose; 1, 3, 5, 7-tetramethylcyclotetrasiloxane and vinyl pentamethyl disiloxane are reacted to obtain a single-end vinyl hydrogen-containing silicone oil; acrylic acid, methyl acrylate, hydroxypropyl methacrylate and the single-end vinyl hydrogen-containing silicone oil are copolymerized to obtain modified acrylic resin; and the modified acrylic resin, the modified cellulose, the modified titanium white powder and various additives are uniformly mixed to prepare the polyurethane automobile finish. The polyurethane automobile finish prepared by the application has excellent quick-drying property, impact resistance and anti-aging property.
Owner:BAOHONG COATINGS (GUANGDONG) CO LTD

A method of preparing enzalutamide

The application belongs to the field of pharmaceutical chemical industry and particularly relates to a preparation method of enzalutamide. In the application, N-BOC-2-aminoisobutyramide is used as a starting material to form a ring with phenyl chlorothioformate to obtain 5,5-dimethyl-1-tert-butoxycarbonyl-2-thione imidazole-4-ketone, the obtained product is further subjected to nucleophilic substitution with 2-trifluoromethyl-4-bromobenzonitrile, is deprotected, and is subjected to nucleophilic substitution with 2-fluoro-4-bromobenzamide to obtain enzalutamide. The method uses N-BOC-2-aminoisobutyramide as a starting material, does not produce disubstituted impurities, has higher conversion rate, can obtain a product with high yield, and is more suitable for industrial amplification.
Owner:SHANDONG NEW TIME PHARMA CO LTD

Method for synthesizing ethyl 4-bromo-5-chloro-2-ethyoxyl benzoate

The invention discloses a process method for synthesizing ethyl 4-bromo-5-chloro-2-ethyoxyl benzoate, and belongs to the technical field of medical intermediates. The method comprises the following steps: by taking 2-fluoro-4-bromoxynil as a raw material, firstly carrying out esterification and ethyoxyl substitution reaction on the 2-fluoro-4-bromoxynil and ethanol to generate 4-bromo-2-ethyoxyl ethyl benzoate, and then carrying out NCS chlorination reaction to generate the 4-bromo-5-chloro-2-ethyoxyl ethyl benzoate. The method has the advantages of originality, good reaction selectivity, high product purity and high yield.
Owner:DALIAN DOUBLE BORON PHARM CHEM CO LTD

Preparation method of hydrobromic acid vortioxetine

The invention discloses a preparation method of hydrobromic acid vortioxetine, and belongs to the technical field of organic synthesis. The method comprises the following steps: by taking o-aminothiophenol and Boc2O as initial raw materials, carrying out amino protection to obtain an intermediate 1; reacting the intermediate 1 with 2, 4-dimethyl bromobenzene under an alkaline condition to form a thioether bond, and acidifying to obtain an intermediate 2; carrying out high-temperature cyclization on the intermediate 2 and bis (2-bromoethyl) amine hydrobromide in mesitylene, so as to obtain a crude product of the hydrobromic acid vortioxetine; and recrystallizing the crude product with 95% ethanol to obtain a high-purity final product. The route is simple, only three-step reaction is needed, a noble metal catalyst is not needed in the whole process, and the problem of metal residues is fundamentally avoided; the selected raw materials are easy to obtain, the reaction condition is mild, the operation is simple and convenient, the process is stable, the total yield is good, the product purity is as high as 99.9%, and the method is suitable for large-scale production.
Owner:SHANDONG JINGJIN PHARM CO LTD

A negative electrode sheet, a method for manufacturing the same, and a lithium ion battery

This invention discloses a negative electrode sheet, its preparation method, and a lithium-ion battery. The negative electrode sheet includes a negative current collector, a first active coating, and a second active coating. The first active coating is located between the negative current collector and the second active coating. The porosity of the second active coating is greater than that of the first active coating. The pores in the second active coating are created by volatilizing volatile solid additives under gradient heating conditions. The volatile solid additives include at least one of 1,8-dichloronaphthalene, 3,5-dichlorobromobenzene, and 1,4-dibromo-2,5-difluorobenzene. The gradient heating includes first gradient heating and then gradient cooling. By using volatile solid additives to create pores through gradient heating and then gradient cooling, this invention provides a negative electrode sheet that balances high areal density and high compaction density, thereby improving the capacity utilization, energy density, and cycle performance of the positive electrode.
Owner:SVOLT ENERGY TECHNOLOGY CO LTD

Porous arylamine polymer stabilizer suitable for nitrocotton

The invention relates to a porous arylamine polymer stabilizer (POP-EDA) suitable for nitrocotton, which is prepared from a node unit 1, 3, 5-tribromobenzene and a connecting unit ethylenediamine. As chain fatty amine, ethylenediamine not only can introduce NOX absorption active sites, but also can construct a non-conjugated spatial network arylamine polymer structure. Compared with a conventional stabilizing agent, the polymer has high thermal stability and a relatively high specific surface area, not only has efficient physical adsorption capacity on nitrogen oxides generated by decomposition of nitrocotton, but also can stably and chemically fix the nitrogen oxides, so that autocatalytic decomposition of the nitrocotton is inhibited, and the service life of the nitrocotton can be effectively prolonged. The problems of poor thermal stability, few reaction active sites, generation of by-product gas, poor stabilizing effect and the like of the existing small-molecule stabilizing agent are solved, and the stability of the nitrate-based energetic material can be widely enhanced.
Owner:NANJING UNIV OF SCI & TECH

Synthesis method of hydroxytyrosol

The invention discloses a synthesis method of hydroxytyrosol. The synthesis method comprises the following steps: (1) reacting p-hydroxyphenethyl alcohol as shown in a formula 1 with a bromination reagent in ethyl acetate at 0-25 DEG C to generate p-hydroxybromophenethyl alcohol as shown in a formula 2; (2) under the protection of nitrogen, reacting p-hydroxybromophenethyl alcohol in an aqueous solution of alkali in the presence of a copper catalyst and a ligand at 80-100 DEG C to generate hydroxytyrosol as shown in a formula 3; the copper catalyst is cuprous bromide; the ligand is phenanthroline. The raw materials and solvents required by the synthesis method are cheap and easy to obtain, the operation process is convenient and easy to implement, the synthesis method is environment-friendly, the reactant yield is high, the quality is good, and the synthesis method is suitable for industrial large-scale production.
Owner:ZHEJIANG UNIV OF TECH

A method for preparing a cyclopentane derivative from a furan compound

PendingCN122404117AFuranChlorobenzene
This invention belongs to the field of catalysis technology, specifically relating to a method for preparing cyclopentane derivatives from furan compounds. The method includes the following steps: mixing a furan compound, a copper-based catalyst, a halogen modifier, and a first solvent, and reacting them under a hydrogen atmosphere; the halogen modifier is at least one selected from sodium chloride, sodium bromide, potassium chloride, potassium bromide, chlorobenzene, and bromobenzene. This invention, by adding a halogen modifier to the catalytic system, introduces halogen components onto the surface of the copper-based catalyst to construct Cu-halogen active centers, achieving highly selective rearrangement of furan compounds into cyclopentane derivatives under relatively mild conditions, while significantly suppressing condensation side reactions, improving carbon utilization efficiency, and reducing dependence on the type of support.
Owner:ZHENGZHOU UNIV

A butyl tin-cyclometalated iridium phenylpyridine complex with AIE characteristics, and a preparation method and application thereof

The application discloses a butyl tin-cycloiridium phenanthroline complex with an aggregation-induced emission (AIE) property, a preparation method of the complex and anticancer application of the complex. The structural formula of the complex is shown as formula (I), and R is one of hydrogen, a phenyl group, a p-tolyl group, a p-bromophenyl group, a p-fluorophenyl group, a biphenyl group, a triphenylamine group, a carbazole group, a tetraphenyl ethene group and a triphenylbenzene group. The growth inhibition rates of the target compound on human alveolar basal epithelial carcinoma cells (A549) and cisplatin-resistant cells (A549 / DDP), cervical cancer cells (Hela) and human lung normal epithelial cells (BEAS-2B) are tested, and it is found through comparison that the target compound shows potential anticancer activity. In addition, the target compound shows unique AIE emission characteristics. The target compound mainly targets the lysosomes of A549 cells, and influences the mitochondria to cause the decline of the mitochondrial membrane potential, thereby showing anticancer activity.
Owner:QUFU NORMAL UNIV

Preparation method of nirapalide tosylate

The invention provides a preparation method of nirapalide tosylate, which is characterized in that 1H-indazole-7-carboxyl methyl ester, 2, 4-dimethoxybenzylamine and (S)-3-(4-bromophenyl) piperidine-1-carboxylic acid tert-butyl ester are used as raw materials to react to prepare the nirapalide tosylate. The method has the advantages of simple process operation, few side reaction products and high purity of the obtained product, and is suitable for industrial production of nirapalide tosylate.
Owner:NANJING WEICHUANGYUAN PHARM TECH CO LTD