14 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 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 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 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 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 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.