715 results about "Bromobenzenes" patented technology

The invention provides adducts comprising a carbon nanotube with covalently attached silane moieties, and methods of making such adducts. Examples of silane moieties include trimethoxysilane; hexaphenyldisilane; silylphosphine; 1,1,1,3,5,5,5-heptamethyltrisiloxane; polydimethylsiloxane, poly(N-bromobenzene-1,3-disulfonamide); N,N,N′,N′-tetrabromobenzene-1,3-disulfonamide; hexamethyldisilazane (HMDS); chlorotrimethylsilane (TMCS); trichloromethylsilane (TCMS); an alkyl(alkylamino)silane; a tri(alkoxy)silane; tert-butyldimethylsilane; monochloroaminosilane; dichloroaminosilane; trichloroaminosilane; and dimethylaminosilane.

The invention provides a method for preparing bromhexine hydrochloride, which comprises the steps as follows: (1) 2-amino-3,5-dibromo benzaldehyde and reducing agents are in a reduction reaction to generate 2-amino-3,5-dibromo benzyl alcohol; (2) 2-amino-3, 5-dibromo benzyl alcohol that is obtained in the step (1) reacts with chlorinating agents to generate 2, 4-bromine-6-chloride methylaniline; and (3) 2,4-bromine-6-chloride methylaniline obtained in the step (2) and N-methylcyclohexylamine are in an amination reaction, and then 2, 4-bromine-6-chloride methylaniline and HCl salification agents are in a salification reaction, so that bromhexine hydrochloride is obtained. The preparation method adopts multiple advanced technologies, is easy to get starting materials, and has the advantages of stable property of intermediates, extremely low environment pollution, high yield coefficient of products and high purity.

The invention belongs to the technical field of electron transport materials and discloses an organic micro-molecular electron transport material and preparation thereof, and an n-doped electron transport layer and application thereof. The organic micro-molecular electron transport material has a structure shown as the formula I. The preparation method of the organic micro-molecular electron transport material comprises (1) subjecting 2-chloro-4, 6-diphenyl-1, 3, 5-triazine and 3-bromo-phenylboronic acid to coupling reaction, and then performing subsequent processing to obtain a bromine-containing intermediate; (2) subjecting the bromine-containing intermediate and bis-(pinacolato)-diboron to Suzuki reaction and then performing subsequent processing to obtain a borate intermediate; (3) subjecting the borate intermediate and 3-bromo-1, 10-phenanthroline to coupling reaction and performing subsequent processing to obtain the organic micro-molecular electron transport material. The organic micro-molecular electron transport material is simple in structure and high in thermostability and topographic stability; when n-doped, the organic micro-molecular electron transport material can beprepared into the n-doped electron transport layer, which achieves high luminous efficiency and stability when applied to organic electroluminescence devices.

The invention discloses a soluble electroluminescent green light organic molecule glass material, a preparation method and applications thereof. The material comprises two types of a symmetric substituent benzothiadiazole derivative and a dissymmetric substituent benzothiadiazole derivative. The preparation method of the material comprises: carbazol and fluorine or anthracene are taken as raw materials, a bromide that contains Ar1 is obtained through palladium-catalyzed coupling reaction or cuprous salt catalyzed coupling reaction, and corresponding boric acid ester is generated through a next reaction; the boric acid ester is reacted with 4, 7-dibromo benzothiadiazole or a bromide of benzothiadiazole substituted by soluble resin Ar2 and a tiny molecule luminescent material which is symmetric or dissymmetric is obtained. The luminescent material prepared has good solubility in a solvent with high boiling point and weak polarity and can be purified by the solution method; simultaneously, the luminescent material has good thermal stability and morphologic stability, particularly the luminescent material with the dissymmetric structure has advantages in both synthesis and purification, thus having important application prospect in electroluminescence display, illumination and laser.

A process for synthesizing pirfenidone from bromobenzene having less than about 0.15% by weight dibromobenze is disclosed. Also disclosed are processes of synthesizing pirfenidone without using ethyl acetate or n-butanol, and pirfenidone having controlled levels of ethyl acetate, n-butanol, di(5-methyl-2-pyridinone)benzenes, and other impurities having specified retention times. Also disclosed are formulated dosage forms including the disclosed pirfenidone.

The invention discloses a method for preparing a fluorine-containing benzoxazole liquid crystal compound. The compound has a structural formula shown in the description, wherein R refers to C2-16 straight-chain paraffin; X, Y and Z refer to respectively independent fluorine or hydrogen, X, Y and Z refer to hydrogen alternatively, and M refers to hydrogen, chlorine or nitro. The preparation method comprises the following steps: by taking 4-hydroxyl fluorinated bromobenzene, 1-bromoalkane and 4-formylphenylboronic acid as reaction raw materials, preparing 4'-alkoxyfluorobiphenylcarboxaldehyde, and reacting 4'-alkoxyfluorobiphenylcarboxaldehyde with aminophenol to prepare the fluorine-containing benzoxazole liquid crystal compound under the action of an oxidant. Compared with the classical method and the improved method, the method has the advantages of fewer steps, simple operation, low cost and high yield and can be used for preparing fluorine-containing benzoxazole liquid crystal.

The invention discloses a method for synthesizing doxylamine succinate. 2-acetylpyridine is taken as an initiative material, and the method comprises the following steps of: reacting the 2-acetylpyridine with a Grignard reagent prepared from bromobenzene and magnesium to obtain 2-pyridyl phenyl methyl carbinol; reacting the 2-pyridyl phenyl methyl carbinol with sodium amide and 2-dimethylaminoethyl chloride in turn to obtain doxylamine; and performing salt-forming reaction on the doxylamine and succinic acid to obtain the doxylamine succinate. The synthesis route is orientation reaction without byproduct. The doxylamine succinate is an ethanol antihistamine, and has antihistaminic and cholinolytic effects and obvious tranquillizing effect.

The invention discloses a preparation method of umeclidinium bromide. The method is suitable for industrial routine reactions, and industrial production schemes exist at present. A technical scheme adopted in the invention is characterized in that a Grignard reagent is adopted to substitute a lithium reagent, bromobenzene, chlorobenzene and other benzene halides are adopted as raw materials, and ether and tetrahydrofuran can be used as a solvent. Compared with the prior art, the method disclosed in the invention has the following advantages: 1, the lithium reagent with high price is substituted by magneson; 2, reaction conditions are mild, too low temperature is not needed, and the reaction temperature is about 0-5DEG C, so the refrigeration cost is reduced; and 3, a routine device can be used, and the Grignard reaction is a classic reaction and industrially exists for a hundred years or above, so people can be simply trained, and the device is mature and has high operating stability.

The invention discloses a synthetic method for 2-methyl-3-trifluoromethyl phenylamine. The method comprises the following steps: 1) preparing 3-nitro-4-methyl benzenesulfonic acid; 2) preparing 3-nitro-4-methyl-5-bromobenzenesulfonic acid; 3) preparing 2-nitro-6-bromotoluene; 4) preparing 2-nitro-6-trichloromethyl toluene; 5) preparing 2-nitro-6-trifluoromethyl toluene; 6) preparing 2-methyl-3-trifluoromethyl phenylamine, that is, adding 5% palladium-charcoal and methanol in 2-nitro-6-trifluoromethyl toluene obtained in step 5), carrying out hydrogenation reduction at a temperature of 35 DEG C and removing a catalyst so as to obtain 2-methyl-3-trifluoromethyl phenylamine. According to the invention, p-toluenesulfonic acid is used as a starting material, and therefore, disadvantages of theprior art are overcome and yield of a target product is improved.

The invention relates to a method for preparing structure type flame-retardant castor-oil-based polyester polyol and applications thereof. The method comprises the following steps: castor oil and small-molecular alcohol generate alcoholysis reaction under the existence of an alkali catalyst, and then generate esterification reaction with tetrabromophthalic anhydride under the existence of an esterification catalyst, and the flame-retardant castor-oil-based polyester polyol is obtained, wherein the hydroxyl value is 100-450mg/gKOH, the acid value is less than or equal to 1.5mg/gKOH and the content of bromine is 5-30wt%. In the method, the middle process does not need to be separated, the cost is low and the process is simple, and the flame retardance of the prepared polyurethane foam is obviously improved. The prepared polyurethane foam has the advantages of no liquid drop of a product in burning, shape maintenance, less smoke density and the like and can be used for buildings, insulation and certain special fields.

The invention belongs to the field of pharmaceutical chemistry and relates to a 1, 2, 3-triazole compound, comprising 4-(2-bromophenyl)-1H-1, 2, 3-triazole and 4-(2-chlorphenyl)-1H-1, 2, 3-triazole. The result of an inhibitory activity test of indoleamine 2, 3-dioxygenase indicates that the disclosed 1, 2, 3-triazole compound used as the indoleamine 2, 3-dioxygenase inhibitor has broad prospect of application and can be applied to the treatment of diseases with indoleamine 2, 3-dioxygenase-mediated tryptophan metabolic pathway pathological characteristics, including cancer, AIDS (Acquired Immure Deficiency Syndrome), Alzheimer disease, tristimania, cataract and other critical diseases.

The invention discloses an aromatic diamine compound containing aryl phosphine groups, a prepration method and an application thereof. The structural general formula of the compound is shown in a formula I. The compound takes 3,5-difluoro-bromobenzene and diphenylphosphinic chloride as raw materials, firstly prepares 3,5-difluorophenyl diphenyl phosphine oxide by Grignard reaction and then continuously reacts with 3-aminophenol for preparation. The compound has smaller steric effect and has great value for improving the heat resistance performance of atomic oxygen resistant polyimide thin film materials and improving the visible light transparency. In addition, polyimide phosphine-containing polymer materials prepared by utilizing the phosphine-containing aromatic diamine compound have good atomic oxygen resistance performance, higher glass transition temperature and better visible light transparency, thereby being capable of being applied in the manufacturing of satellites and other aircraft parts in the LEO environment.

The invention relates to a preparation method of a graphdiyne-loaded monatomic catalyst, which belongs to the technical field of preparation of monatomic catalysts. The technical problems of atom aggregation and carrier structure damage easily caused by instability of existing metal monatomic and carrier materials at continuous high temperature is solved. The method comprises the steps of 1 mixinghexabromobenzene and calcium carbide, dissolving in ethanol, and grinding; 2 centrifuging, washing and calcining the generated reaction product; 3 carrying out acid washing treatment on the calcinedproduct to obtain graphdiyne; 4 soaking graphdiyne in a metal precursor solution to obtain graphdiyne loaded with a metal precursor; and 5 carrying out joule heating treatment on the graphdiyne loadedwith the metal precursor to a certain temperature to obtain the graphdiyne-loaded metal monoatomic catalyst. The monoatomic catalyst prepared by the method can prevent continuous high temperature from damaging the stability of the catalyst carrier, and atom aggregation is avoided.

The invention discloses a microporous polymer-nano-metal particle catalyst and especially relates to a microporous polymer-nano-palladium catalyst and a preparation method thereof. The preparation method comprises that prepared bromine-substituted triarylimidazole group-containing monomer 2, 4, 5-tris(4-bromophenyl)-1-alkylimidazole (TAI) undergoes a reaction to produce a microporous polymer, the microporous polymer is dissolved in DMF, and an appropriate amount of a H2PdCl4 aqueous solution is added into the DMF solution and undergoes a reaction, and excess NaBH4 is added into the reaction product so that the microporous polymer-nano-metal particle catalyst is obtained. The microporous polymer has high nitrogen content, has a multi-pore structure and helps to increase the loading amount of the transition metal. The catalyst has strong catalytic activity, good selectivity, mild reaction conditions, good reusability and a good market application value.

The invention discloses an elastic hydrophobic organic conjugated polymer, a synthesizing method thereof and an application thereof to removing of organic matters from water. The synthesizing method comprises the following steps of: connecting a benzene ring with an acetylene bond; particularly adding a catalyst, a nonpolar solvent and the like into 1.4-diacetylene-benzene and a 1,3,5-tribromobenzene derivative or a 1,3,5-triiodo benzene derivative serving as substrates in an inert atmosphere; undergoing a polymerization reaction; and filtering, washing, drying and the like to obtain a product. The product is centimeter grade or millimeter grade elastic particles containing a plenty of mesopores and gaps, so that material density is very low; and meanwhile, the copolymer has high elasticity and high hydrophobic property. When adsorption of liquid organic matters is saturated in the polymer, the polymer is taken out of an aqueous solution, organic matters are removed through mechanicalextrusion, and polymer particles can be used repeatedly, so that the cost on removal of the organic matters from water is lowered. The elastic hydrophobic organic conjugated polymer is suitable for batch production and environmental protection.

The invention discloses thiophene polycyclic organic semiconductor material synthesis based on pyrene and belongs to the field of photoelectric conversion materials. The molecular formulas of compounds are C<76>H<86>N<4>S<4> and C<62>H<80>N<2>S<2>, and the structural formula can be seen in the Application of the invention. A synthesis method comprises the steps of making the pyrene react with liquid bromine, and obtaining 1,3,6,8-tetrabromo pyrene; making the 1,3,6,8-tetrabromo pyrene react with 1-octyne, obtaining a product, and then using palladium/carbon for conducting catalytic reaction,and obtaining 1,3,6,8-quadri-octane pyrene; using ruthenium trichloride for catalyzing the 1,3,6,8-quadri-octane pyrene, adjusting the using amount of sodium periodate, and obtaining tetrone and diketone; then making o-phenylenediamine and sulfoxide chloride react with liquid bromine, and obtaining 4,7-dibromo-2,1,3-diazosulfide; making thiophene react with thiadiazole, and obtaining diazosulfide; then making o-phenylenediamine and paratoluensulfonyl chloride react with liquid bromine, subsequently, making the mixture react with concentrated sulfuric acid, then making the mixture react with thionyl chloride, and obtaining 5,6-dibromo-2,1,3-diazosulfide; conducting operation same with the reaction process, and obtaining another type of diazosulfide; making a thiadiazole product to be subjected to ring-opening reaction, and obtaining two types of o-phenylenediamine products; making the tetrone and the diketone react with the two types of o-phenylenediamine respectively, and obtaining the compounds.

The invention provides arylboronic acid derivatives and a preparation method thereof. The two arylboronic acid derivatives are tri(4,4',4'-triboric acid-phenyl)amino(3BzN-3B) and tri(4,4',4'-triboric acid-phenyl)boron(3BzB-3B), and the molecular structures are as shown in the specification. 3BzN-3B and 3BzB-3B are prepared by firstly, respectively reacting tri(4,4',4'-triboric acid-phenyl)amino and tri(4,4',4'-triboric acid-phenyl)boron with n-butyllithium, secondly, respectively carrying out nucleophilic substitution reaction with boric acid ester, and finally carrying out acidolysis by using diluted hydrochloric acid. The products of the arylboronic acid derivatives, namely, the 3BzN-3B and the 3BzB-3B are expected to be excellent environment-friendly organic fire retardants.

The invention discloses a method for preparing 4-amino benzene boric acid hydrochloride. The method comprises the steps that 1), catechol and 4-nitrobromobenzene are subjected to a reaction for 2-3h in a polar solvent under the action of potassium acetate and Pd (dppf) C12, the temperature is lowered to a room temperature, filtering is performed, ethyl acetate is extracted, and a crude product is pulped and filtered through nonpolar varsol after an organic layer is concentrated, so that 4-nitrophenylboronic acid is obtained; and 2), the 4-nitrophenylboronic acid is subjected to palladium carbon catalytic hydrogenation in the ethyl acetate, hydrogenation is performed for 6-8h at the temperature ranging between 60 DEG C and 80 DEG C and under 0.8-1.0 MPa, filtering is performed at the temperature of 15-25 DEGC after the reaction, concentrated hydrochloric acid is added into the filtering liquid at the temperature of 0-10 DEG C, filtering is performed, and the crude product is obtained, then pulped with acetone, filtered and dried, so that the 4-amino benzene boric acid hydrochloride is obtained. According to the method, raw materials are low in toxicity and can be processed easily, copious cooling and low temperature are avoided simultaneously, the reaction temperature can be reached easily, the conditions are mild, the yield is high, the process is safe and reliable, and method is suitable for industrial production.

The invention relates to preparation of (S)-1-(4-methoxy-3-ethoxy)phenyl-2-methylsulfonyl ethylamine and a preparation method of apremilast. 4-methoxy-3-ethoxy phenylmagnesium bromide is prepared from 4-methoxy-3-ethoxy bromobenzene through Grignard reaction; 4-methoxy-3-ethoxy phenylmagnesium bromide is in addition reaction with methylsulfonyl acetonitrile, and then hydrolysis and reduction are carried out, so that (R,S)-1-(4-methoxy-3-ethoxy)phenyl-2-methylsulfonyl ethylamine (III) is obtained; separation and filtering are carried out, so that (S)-1-(4-methoxy-3-ethoxy)phenyl-2-methylsulfonyl ethylamine N-acetyl-L-leucine salt (IV) is obtained; through neutralization, (S)-1-(4-methoxy-3-ethoxy)phenyl-2-methylsulfonyl ethylamine (II) is obtained; the compound (II) is subjected to imidization, so that apremilast (1) is obtained. The mother liquor obtained after separation is recycled and converted into a compound IV, so that discharge of waste liquid is reduced, environment friendliness is realized and the cost is reduced.

The invention belongs to the technical field of new drug synthesis, in particular to a class of 4-amino-6-(3-(3-bromophenyl)phenyl)-5-cyano-7-(β-L-xylofuranose)pyrrolo [2,3-d]pyrimidine, its similar derivatives, and drugs for preparing anti-human liver cancer cells, human lung cancer cells, human breast cancer cells, human cervical cancer cells, and human gastric cancer cells. The compounds of the present invention are directed against 4-amino-6-(3-(3-bromophenyl)phenyl)-5-cyano-7-(β-L-xylofuranose)pyrrolo[2,3 -d] The C6 position of pyrimidine is modified and synthesized by chemical methods. Experiments have shown that this type of compound can significantly inhibit the proliferation of various cancer cells, effectively induce apoptosis of cancer cells, including highly metastatic cancer cells, and can be used as drugs and drug components for treating cancer.

The invention relates to a recoverable ligand-free mesoporous polymer palladium catalyst and a synthetic method and application thereof. The catalyst has a two-dimensional hexagonal ordered mesostructure. specific surface area is 250-380 m<2>/g; pore diameter is 3.0-7.0 nm; mass content of a functional phase transfer agent is 8.5-13 wt%; mass content of metal palladium is 1-5 wt%; and particle size of palladium particles is 3-5 nm. The preparation comprises the following steps: adding a surfactant and hydrochloric acid into an organic solvent, stirring and reacting, successively adding a silicon source, quaternary ammonium salt and a carbon source, continuously stirring and reacting; carrying out a thermosetting reaction, and then carrying out high-temperature calcining to prepare a functional mesoporous polymer carrier; and mixing the functional mesoporous polymer carrier and a palladium source, stirring, carrying out suction filtration, washing, carrying out vacuum drying, and carrying out a reduction reaction. The catalyst is applied in aqueous medium catalysis of a Heck reaction between bromobenzene and styrene for generation of stilbene. In comparison with the prior art, the method of the invention is simple; and the catalyst is efficient and stable, can be recycled for many times and has a wide application prospect in the field of industrial catalysis.

The invention discloses a novel two-dimensional covalent organic framework material and preparation and application thereof, belongs to the field of new energy, and particularly relates to an organicframework material and preparation and application thereof. The two-dimensional covalent organic framework material is prepared by the following steps: carrying out Sonogashira coupling reaction and deprotection on a benzene compound 1, 3, 5-tri (4-bromophenyl) benzene containing bromine atoms, and finally, carrying out Schiff base reaction on the product and a tert-butyloxycarbonyl protecting group. The covalent organic framework material is low in raw material cost, simple in synthesis process and convenient to purify. When the covalent organic framework material is used as a proton exchangemembrane, the battery can keep excellent voltage working stability in a normal operation state; when the current density is 188mA/cm <2 >, the power density of the fuel cell is maximum and reaches 72mw/cm <2 >, and the fuel cell has higher power density at room temperature.