22 results about "Boron tribromide" patented technology

The present application relates to the field of medicine synthesis, and discloses a preparation method and application of brominated piperonal carboxylic acid, wherein the brominated piperonal carboxylic acid compound is prepared from o-vanillin as a starting material through acetyl protection, bromination reaction, deprotection and demethylation reaction, cyclization reaction and Pinnick oxidation reaction.No longer through a brominated piperonal intermediate, and without using a live LDA reagent low-temperature lithiation reaction, the safety and stability are greatly improved.The deprotection and demethylation reaction is carried out in one pot, and the use of boron tribromide and other reagents is avoided;finally, the oxidation step from aldehyde to acid avoids using traditional silver oxide or potassium permanganate oxidation, and adopts Pinnick oxidation, which is economic, environmental protection and cost reduction, and greatly improves the yield.The whole has the advantages of easy-to-obtain raw materials, short steps, mild reaction conditions, low production cost, environmental protection, high yield and high purity, and can meet the high quality requirements of pharmaceutical products.

The invention discloses a preparation method of a cyanoborate lithium salt derivative, which comprises the following steps: 1, mixing an alcohol compound, a lithium source compound, a boron source compound and trimethylsilyl cyanide in a polar organic solvent, and filtering after complete reaction to obtain a cyanoborate crude product filtrate; the alcohol compound is selected from one of 2, 2, 2-trifluoroethanol, 2, 2-difluoroethanol, 2-fluoroethanol, 3-hydroxypropionitrile, allyl alcohol and propargyl alcohol; the lithium source compound is selected from one of lithium carbonate and lithium hydroxide; the boron source compound is selected from one of boric acid, diboron trioxide and boron tribromide; the reaction temperature is controlled to be 0-120 DEG C; and 2, adding an inert organic solvent into the cyanoborate crude product filtrate for crystallization, and performing vacuum drying to obtain a finished product of the cyanoborate lithium salt. The method has the advantages of high yield and purity, simple process, convenience in operation and low cost, and is extremely suitable for industrial production.

The invention belongs to the technical field of zinc ion batteries, and particularly relates to a hexahydroxy truxene organic positive electrode material for an aqueous zinc ion battery, a preparation method and application. According to the method, 5, 6-dimethoxy indanone is taken as a raw material, p-toluenesulfonic acid is taken as a catalyst, ethylene glycol is taken as a cocatalyst, 2, 3, 7, 8, 12, 13-hexamethoxy truxene is efficiently synthesized through a water diversion reflux reaction, and then a target product 2, 3, 7, 8, 12, 13-hexahydroxy truxene is obtained through a boron tribromide demethylation reaction. According to the method, the defect that a traditional polyphosphate (PPE) catalyst synthesis process is tedious is overcome, meanwhile, the technical problem that a trimerization product cannot be prepared by replacing an acid catalyst is solved, and the prepared hexahydroxy truxene material is of a nanorod-shaped structure, has excellent cycling stability and high specific capacity when serving as an aqueous zinc ion battery positive electrode material and is suitable for being used as a water-based zinc ion battery positive electrode material. The material can adapt to high-rate charge and discharge, and the overall electrochemical performance is excellent.

The invention relates to a compound MDMB-BUTINACA-D3 as well as preparation and application thereof, and the structural formula of the compound MDMB-BUTINACA-D3 is as follows: 2-(1H-indazole-3-formamido)-3, 3, 4-triazole-3-carboxylic acid is obtained through condensation reaction of indazole-3-carboxylic acid and tert-leucine methyl ester hydrochloride; the preparation method comprises the following steps: adding 2-(1H-indazole-3-formamido)-3, 3-dimethyl butyric acid methyl ester into 2-(1H-indazole-3-formamido)-3, 3-dimethyl butyric acid methyl ester, adding 3-phenoxybromopropane into a Grignard reagent, carrying out a substitution reaction to obtain butoxybenzene-D4, further adding a brominating agent boron tribromide, carrying out a bromination reaction to obtain bromobutane-D3, and finally carrying out a substitution reaction on 2-(1H-indazole-3-formamido)-3, 3-dimethyl butyric acid methyl ester and bromobutane-D3 again to obtain MDMB-BUTINACA-D3. According to the method, the matrix effect can be well avoided, meanwhile, mass spectrum cross signal overlapping caused by natural isotopes can be avoided, and the mass spectrum quantitative analysis precision can be remarkably improved when the method is used as an internal standard substance for MS quantitative determination.

The invention relates to the technical field of conductive coatings, in particular to an aircraft fairing surface conductive coating and a preparation method thereof. The conductive coating is prepared from the following raw materials: conductive phthalonitrile, N, N-dimethylformamide, a dispersing agent BYK-110, 3-aminopropyltriethoxysilane, a flatting agent BYK-333 and a de-foaming agent BYK-066N; wherein the conductive phthalonitrile is prepared by the following steps: removing methoxyl by boron tribromide to prepare a hydroxyl thienopyrroledione intermediate, then reacting 5-bromo-2-fluoroaniline with 4, 4-dihydroxyl stilbene to obtain a monomer A, and subsequently reacting with hydroxyl thienopyrroledione and 4-nitro-2-trifluoromethyl-phthalonitrile to purify, thereby obtaining the conductive phthalonitrile. After the paint is prepared, a coating is formed through stepped heating curing and three-time spraying. The conductive coating achieves accurate balance of static dissipation and radar permeability, is compact in structure and high in adhesive force, can resist high and low temperature circulation and salt spray corrosion, and has excellent performance and engineering practicability.

The invention discloses an alkyl-substituted free radical polymer based on 3, 4-dimethoxythiophene and a preparation method of the alkyl-substituted free radical polymer. The preparation method comprises the following steps: dissolving 3, 4-dimethoxythiophene in an organic solvent A, adding an aldehyde substance and boron trifluoride diethyl etherate, heating to 50-120 DEG C, and reacting for 2-20 hours; after the reaction is finished, quenching, extracting with an organic solvent B which is immiscible with water, collecting an organic phase, concentrating, purifying, and filtering, washing and drying the obtained product to obtain a polymer intermediate; dissolving the polymer intermediate in an organic solvent E, stirring at normal temperature, adding boron tribromide, and reacting for 0.5-12 hours; and after the reaction, quenching, filtering, washing and drying. The polymer disclosed by the invention has a strong free radical effect, is beneficial to improving the ionic conductivity and mobility, and can be applied to the fields of coating layers of organic photoelectric devices and lithium ion battery positive electrode materials and the like.

The novel vaporization kettle for boron tribromide processing comprises a kettle body, a protective shell is arranged on the outer side of the kettle body, supporting legs are connected to the two sides of the bottom of the protective shell, and a heat preservation plate is laid on the inner side wall of the protective shell; the two sides of the bottom of the kettle body are connected with the inner bottom of the protective shell through a base, the left upper end of the kettle body is connected with a gas exhaust pipeline, a feeding pipeline is inserted into the right upper end of the kettle body, and the upper end of the gas exhaust pipeline sequentially penetrates through a heat preservation plate and the protective shell from bottom to top and extends upwards; the upper end of the feeding pipeline sequentially penetrates through the heat preservation plate and the protective shell from bottom to top and extends upwards. According to the vaporization kettle, the heat preservation plate, the protective shell and the supporting legs are arranged and are matched with one another, so that the heat preservation and heat insulation performance of the vaporization kettle is improved, heat dissipation is slow, and the energy-saving effect is achieved.

The invention discloses a novel synthetic method of naphthazarin, which comprises the following steps of: 1, reacting 1, 4, 5, 8-tetramethoxynaphthalene with boron tribromide or aluminum trichloride, crystallizing to obtain a high-purity product, and distilling a solvent under reduced pressure to obtain 5, 8-dihydroxy-2, 3-dihydronaphthalene-1, 4-diketone; 2, 5, 8-dihydroxy-2, 3-dihydronaphthalene-1, 4-diketone is added into another reaction kettle, an alkali solution is added, an oxygen micro-positive pressure (0.01-0.03 MPa) is performed for a reaction, and after the reaction is finished, high-purity 5, 8-dihydroxy-2, 3-dihydronaphthalene-1, 4-diketone salt is obtained through ethanol crystallization and filtration; and adding the salt of the 5, 8-dihydroxy-2, 3-dihydronaphthalene-1, 4-diketone into another reaction kettle, adding a hydrochloric acid ethyl acetate solution, heating and reacting, and then filtering and pulping to obtain a final product. The total preparation yield gt of naphthazarin; the HPLC purity is gt; the yield is 99.6%. The route is simple and convenient to operate and easy to implement, raw materials are cheap and easy to obtain, reaction conditions are mild, high-temperature and high-pressure reaction is not needed, and requirements on equipment are reduced. The whole route is safer to the environment, and green and pollution-free production can be realized.

The invention relates to a piperidine functionalized ring-containing polyfluorene ether ketone anion exchange membrane and a preparation method thereof. The preparation method comprises the following steps: reacting tetramethyl bisphenol fluorene with excessive 4, 4 '-difluorobenzophenone to generate an ABA type compound containing four methyl groups, performing cyclization reaction on the ABA type compound and tetramethyl dimethoxy bisphenol fluorene in a dilute solution to obtain a dimethoxy group-containing cyclic compound, reacting the dimethoxy group-containing cyclic compound with boron tribromide to prepare a cyclic monomer containing two phenolic hydroxyl groups, and reacting the cyclic monomer with 4, 4'-difluorobenzophenone to obtain a dimethoxy group-containing cyclic monomer. The preparation method comprises the following steps: carrying out polycondensation on 4, 4 '-difluorobenzophenone and bisphenol fluorene at a high temperature to prepare a ring-containing polyfluorene ether ketone compound, brominating methyl in the ring-containing polyfluorene ether ketone compound by utilizing bromination reaction, reacting with N-methylpiperidine to prepare a piperidine functionalized ring-containing polyfluorene ether ketone compound, and carrying out solution casting to obtain the anion exchange membrane. The obtained anion exchange membrane has the advantages of high ion conductivity, low vanadium ion permeability, high mechanical strength and the like.

The invention discloses a synthetic method of (R)-glabridin with high optical purity, and belongs to the technical field of organic synthesis. The synthesis method provided by the invention comprises the following steps: dissolving methyl-protected isoflavone in a solvent, and adding boron tribromide to carry out a protecting group removal reaction; then carrying out asymmetric hydrogen transfer reaction on a reaction product in an acid-base mixed solution under the action of a chiral ruthenium catalyst; and finally, in the presence of acid, carrying out dehydroxylation reaction on the reaction product and a silane reagent in a solvent to obtain the (R)-glabridin. The (R)-glabridin is efficiently synthesized with high selectivity through a simple three-step reaction, the total yield is high, the optical purity is excellent, the conditions are mild, the post-treatment method is simple, and the method is suitable for large-scale production.

The invention discloses a synthetic method of bisabolane sesquiterpenes and derivatives thereof, and belongs to the technical field of chemical synthesis. The preparation method comprises the following steps: carrying out MOM protection on a phenolic hydroxyl group by using a cheap and easily available compound 1, carrying out benzyl bromination, sodium acetate hydrolysis, benzyl alcohol MOM protection, Grignard reagent addition and Burge reagent elimination, and removing an MOM protecting group under an HCl condition to obtain the natural product Aspergillus A. The method comprises the following steps: carrying out Wolff-Kishner-Huang reduction on a cheap and easily available compound 10, removing a methyl protecting group by using boron tribromide, and carrying out MOM protection on a phenolic hydroxyl group to obtain a compound 13; the preparation method comprises the following steps: carrying out benzyl bromination on a compound 6, carrying out Negishi coupling reaction on the compound 6 and a compound 13, carrying out 1, 2 addition and Burge reagent elimination, and simultaneously removing an MOM protecting group to obtain the natural product YHB-17. Similarly, the natural product YHB-14 is obtained by using the method. A brand new synthesis strategy is used, reaction repeatability is high, operability is good, and the requirement of large-scale industrial production can be met.

This invention relates to the field of selective hydroxylation technology for aromatic compounds, specifically to a boron-mediated hydroxylation method for 1-phenylpyrazole compounds, comprising the following steps: under the action of boron trihalide, a base, and an oxidizing agent, the 1-phenylpyrazole compound represented by formula (I) undergoes a C-H bond borination reaction with boron trihalide, followed by an oxidation reaction to obtain the compound represented by formula (II); wherein, R 1 and R 2 Individually selected from hydrogen, C1-C6 alkyl groups, phenoxy groups, N,N-dimethyl groups, halogens, thiophene groups, and C6-C6 groups respectively. 14 Any of the aryl groups. This invention does not use any metal catalysis. By coordinating boron tribromide with the directing group pyrazole, the 1-phenylpyrazole substrate first undergoes a C-H bond borylation reaction, and then, under the action of an oxidant, a series of 1-(2-hydroxy)-1H-pyrazole compounds are obtained. This method is efficient, low-cost, and environmentally friendly.

This invention relates to a method for preparing a polyester membrane based on perhydroxyl column[5] aromatics. A polyester membrane for dye-salt separation is prepared by interfacial polymerization using perhydroxyl column[5] aromatics as the aqueous monomer. The steps include: (1) synthesizing methoxyl column[5] aromatics from 1,4-dimethoxybenzene and paraformaldehyde under the catalysis of boron trifluoride ether; (2) reacting the purified product with boron tribromide to remove methyl groups and obtain perhydroxyl column[5] aromatics; (3) dissolving the product in an aqueous solution containing triethylamine, and forming a two-phase solution for interfacial polymerization with a hexane solution of trimesoyl chloride; (4) sequentially coating the aqueous solution and organic solution onto the surface of a polyacrylonitrile ultrafiltration membrane, and obtaining the polyester membrane through interfacial polymerization. Based on the inherent cavity and polyhydroxyl characteristics of perhydroxyl column[5] aromatics, compared with traditional polyamide membranes, the obtained polyester membrane has both high permeability and selectivity, and can efficiently separate dyes and inorganic salts, making it suitable for water treatment processes such as dyeing and printing wastewater.

The present invention discloses a method for preparing a water-soluble fluorescent naphthyl[3]arene and its application. The method comprises the following steps: demethylating the naphthyl[3]arene with boron tribromide to obtain a fully hydroxy-substituted naphthyl[3]arene (compound 2); subsequently reacting the compound with tert-butyl bromoalkyl acid to obtain a fully ester-substituted naphthyl[3]arene (compound 3); subsequently hydrolyzing compound 3 with trifluoroacetic acid to obtain a fully carboxylic acid-substituted naphthyl[3]arene; and finally, dissolving the fully sodium carboxylate-substituted naphthyl[3]arene by adjusting the pH. The method prepares a fully sodium carboxylate-substituted naphthyl[3]arene and its application in detecting paraquat. As a supramolecular macrocyclic aromatic hydrocarbon fluorescent probe, the compound has the advantages of simple synthesis, low cost, good selectivity, high sensitivity, and can be used for rapid detection of paraquat and its derivatives in water.

The invention belongs to the technical field of organic synthesis, and discloses a preparation method and application of a metal-free 1-hydroxycarbazole derivative. The preparation method of the 1-hydroxycarbazole derivative comprises the following steps: (1) mixing a compound I and an organic solvent I, adding sodium hydride under an ice bath condition, heating and mixing, then adding R1COCl, and mixing to obtain a mixture a; (2) removing the organic solvent I in the mixture a, adding an organic solvent II and a dichloromethane solution of boron tribromide into the mixture a in a protective gas atmosphere, and reacting to obtain a mixture b; and (3) removing the organic solvent II in the mixture b, adding sodium perborate tetrahydrate and a potassium carbonate solution into the mixture b, mixing, extracting, drying and concentrating to obtain the 1-hydroxy carbazole derivative. The structural formula of the compound I is shown in the specification; the preparation method is free of transition metal catalysis and low in cost, and the yield of the obtained 1-hydroxycarbazole derivative is high.

This invention relates to the field of organic synthesis technology and discloses a method for synthesizing the natural molecule 5-(4-hydroxybenzofuran-2-yl)benzene-1,3-diphenol. 2-Bromo-1,3-dimethoxybenzene and 3,5-dimethoxyacetophenone react under a nitrogen atmosphere with sodium tert-butoxide and methanesulfonic acid (2-dicyclohexylphosphino-2',4',6'-tris-isopropyl-1,1'-biphenyl)(2'-amino-1,1'-biphenyl-2-yl)palladium(II) to generate 2-(2,6-dimethoxyphenyl)-1-(3,5-dimethoxyphenyl)ethane-1-one. Subsequently, a demethylation and cyclization tandem reaction occurs under the action of boron tribromide to generate 5-(4-hydroxybenzofuran-2-yl)benzene-1,3-diphenol. The method of this invention requires inexpensive and readily available raw materials, is simple, has mild reaction conditions, and a high overall yield, making it suitable for industrial-scale preparation.

The invention relates to a sulfonated polyfluorene ether ketone proton exchange membrane containing an aromatic macrocyclic structure and a preparation method of the sulfonated polyfluorene ether ketone proton exchange membrane. The preparation method comprises the following steps: reacting bisphenol fluorene with excessive 4, 4 '-difluorobenzophenone to prepare a fluorine-terminated ABA type compound, reacting with dimethoxy bisphenol fluorene in a dilute solution to prepare a dimethoxy-containing cyclic compound, reacting with boron tribromide to prepare a phenolic hydroxyl group-containing cyclic monomer, and reacting with bisphenol fluorene and 3, 3'-sodium disulfonate-4, 4 '-difluorobenzophenone to prepare a phenolic hydroxyl group-containing cyclic monomer. The preparation method comprises the following steps: carrying out polycondensation on 4, 4 '-difluorobenzophenone and 4, 4'-difluorobenzophenone at a high temperature to obtain a polyarylether compound containing an aromatic macrocyclic structure, and finally carrying out solution casting to form a membrane so as to prepare the proton exchange membrane. The obtained membrane has the advantages of excellent proton conductivity, thermal stability, mechanical property and the like.

The present application relates to a kind of preparation method of flubendiamide intermediate 3 ', 4 ', 5 '-trifluorobiphenyl-2-amine, belong to the technical field of pesticide.The present application with common industrial product acetanilide as starting material, with boron tribromide to generate 2-acetamidobenzoic acid, then with 3, 4, 5-trifluorobromobenzene through nickel catalyst coupling reaction to obtain N-(3 ', 4 ', 5 '-trifluoro [1, 1 '-biphenyl] -2-yl) acetamide, finally through acid or base hydrolysis reaction to obtain flubendiamide key intermediate 3 ', 4 ', 5 '-trifluorobiphenyl-2-amine.The intermediate 2-acetamidobenzoic acid of preparation in the present application does not use palladium catalyst to prepare boric acid, also need not add phase transfer catalyst, reaction does not use polar organic solvent, can be continuous production, suitable for industrial scale production, with the advantages such as simple process, high yield, high production efficiency and green environmental protection.

The invention discloses a colorimetric-fluorescent dual-channel near-infrared probe for H2S specific detection, and a preparation method and application thereof, and belongs to the field of chemical analysis and detection. The preparation method comprises the following steps: firstly, preparing a compound 1 by taking anhydrous N, N-dimethylformamide, dichloromethane, phosphorus tribromide and cyclohexanone as reaction raw materials; reacting the compound 1, cesium carbonate and 2-hydroxy-4-methoxybenzaldehyde to prepare a compound 2; secondly, dropwise adding boron tribromide into a dichloromethane solution in which the compound 2 is dissolved, and reacting to obtain a compound 3; the preparation method comprises the following steps: enabling 3-hydroxy-3-methyl-2-butanone, malononitrile and sodium ethoxide to react to obtain TCF; thirdly, the compound 3 and TCF are subjected to a dissolution reaction, and TEC-OH is obtained; and finally, dropwise adding a dichloromethane solution containing 2, 4-dinitrofluorobenzene into a dichloromethane solution containing TEC-OH and triethylamine, and reacting to obtain the probe TEC-H2S. The colorimetric-fluorescent near-infrared probe TEC-H2S is successfully designed and synthesized on the basis of an intramolecular charge transfer (ICT) mechanism and is used for specific detection of H2S, and a sensing technology with a great application prospect is provided for H2S detection.

This invention discloses a color-changing polyimide ether ketone polymer, its preparation method, and its applications, belonging to the technical field of color-changing material preparation. The preparation method involves: reacting 4,4'-dimethoxydiphenylamine with boron tribromide to synthesize 4,4'-dihydroxydiphenylamine; reacting p-bromobenzoyl chloride, anhydrous aluminum chloride, and fluorobenzene to synthesize 4-bromo-4'-fluorobenzophenone; reacting 4-bromo-4'-fluorobenzophenone, p-phenylenediamine, sodium tert-butoxide, Pd2(dba)3 catalyst, and BINAP under heat to obtain bis(4-fluorophenylbenzophenone)-4,4'-iminodiphenylamine; and reacting 4,4'-dihydroxydiphenylamine, bis(4-fluorophenylbenzophenone)-4,4'-iminodiphenylamine, and anhydrous potassium carbonate under heat to obtain the polyimide ether ketone polymer. This color-changing material exhibits excellent thermal stability, and the synthesis route is simple and easy to operate, effectively solving the problems existing in the prior art.

The invention relates to the technical field of organic synthesis, and discloses a synthesis method of a natural molecule 5-(4-hydroxybenzofuran-2-yl) benzene-1, 3-diphenol, 2-bromo-1, 3-dimethoxybenzene and 3, 5-dimethoxyacetophenone are subjected to a reaction in sodium tert-butoxide and methane sulfonic acid (2-dicyclohexylphosphine-2 ', 4', 6 '-tri-isopropyl-1, 1'-biphenyl) (2 '-amino-1, 3-diphenol), and the reaction product is subjected to a reaction in a solvent to obtain the natural molecule 5-(4-hydroxybenzofuran-2-yl) benzene-1, 3-diphenol. The preparation method comprises the following steps: reacting 2-(2, 6-dimethoxyphenyl)-1-(3, 5-dimethoxyphenyl) ethane-1-ketone in a nitrogen atmosphere under the action of 1, 1 '-biphenyl-2-yl) palladium (II) to generate 2-(2, 6-dimethoxyphenyl)-1-(3, 5-dimethoxyphenyl) ethane-1-ketone; and then carrying out demethylation and cyclization cascade reaction under the action of boron tribromide to generate the 5-(4-hydroxybenzofuran-2-yl) benzene-1, 3-diphenol. The method has the advantages of cheap and easily available raw materials, simple method, mild reaction conditions and high total yield, and is convenient for industrial preparation.