239 results about "P-hydroxybenzaldehyde" patented technology

The invention relates to a phosphorus-containing fire retardant, a preparation method of the phosphorus-containing fire retardant and a flame-retardant epoxy resin prepared from the phosphorus-containing fire retardant, and especially relates to a phosphorus-containing nitrile/DOPO double-base structure phosphorus-containing fire retardant, a preparation method of the phosphorus-containing nitrile/DOPO double-base structure phosphorus-containing fire retardant, and flame-retardant epoxy resin prepared from the phosphorus-containing nitrile/DOPO double-base structure phosphorus-containing fire retardant. The flame-retardant epoxy resin solves the problem that the existing epoxy resin has low flame retardation efficiency and poor compatibility between a polymer matrix and a fire retardant. The preparation method comprises the following steps of 1, dissolving p-hydroxybenzaldehyde and tetrahydrofuran, adding triethylamine into the solution and carrying out stirring, 2, dissolving phosphonitrilic chloride trimer in tetrahydrofuran, dropwisely adding the solution into the reaction system, and carrying out heating and stirring, 3, cooling the reaction system, concentrating the filtrate, pouring the filtrate into water for precipitate separation, carrying out pumping filtration, carrying out recrystallization on the precipitates and carrying out drying to obtain intermediates, and 4, dissolving the intermediates by a solvent, adding p-aminophenol into the solution, carrying out heating reflux, adding DOPO into the reflux product, carrying out condensation, pouring the concentrate into cold ethanol for solid precipitation, and washing and drying the solids to obtain the phosphorus-containing nitrile/DOPO double-base structure phosphorus-containing fire retardant. The flame-retardant epoxy resin comprises epoxy resin, a curing agent and the phosphorus-containing nitrile/DOPO double-base structure phosphorus-containing fire retardant. The preparation method is used for preparing the phosphorus-containing nitrile/DOPO double-base structure phosphorus-containing fire retardant.

The invention relates to an oxa-phosphaphenanthrene flame retardant containing cyclotriphosphonitrile structure, and a preparation method and application thereof. The preparation method comprises the following steps: under the actions of K2CO3 and acetone, reacting hexachlorocyclotriphosphonitrile and 2,2'-diphenyldiphenol to obtain an intermediate I, reacting the intermediate I with p-hydroxybenzaldehyde to obtain an intermediate II, and reacting the intermediate II and DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) to obtain the target compound. The appearance of the compound is white, and the melting point is 186-188 DEG C; and the product has the advantages of favorable thermal stability, high flame retardancy and high purity (up to 99%). The invention has the advantages ofaccessible raw materials and advanced technique, and can easily implement industrial production. The flame retardant can be used as a reactive flame retardant to be connected to epoxy resin, polyurethane and other thermosetting resins, and can also be used as an additive flame retardant for halogen-free flame retardancy of ABS (acrylonitrile-butadiene-styrene), nylon and other engineering plastics with high heat resistance requirements.

The invention discloses an isophorone fluorescence probe, and a preparation method and an application thereof. The structure of the fluorescence probe is represented by formula I. The preparation method comprises the following steps: adding isophorone, malononitrile and pyridine to a reaction bottle, carrying out heating refluxing under the protection of an inert gas for 18-24h, purifying, adding the above obtained pure product, p-hydroxybenzaldehyde and pyridine to the reaction bottle, carrying out heating refluxing under the protection of the inert gas for 4-18h, purifying, adding the obtained pure product, 2,4-dinitrofluorobenzene and triethylamine to the reaction bottle, stirring above materials for 8-36h, and purifying the obtained mixture to obtain the fluorescence probe. The fluorescence probe has large Stokes shift (182nm), long fluorescence emission wavelength (592nm), high sensitivity and good selectivity, can specifically detect hydrogen sulfide in organisms, environment and foods, has good biomembrane permeability and low cytotoxicity, and also has the advantages of simple synthesis route, high yield and very large practical values.

Disclosed is a Sofalcone preparation method which mainly comprises, (1) subjecting p-hydroxybenzaldehyde and 2,4-ihydroxyacetophenone to condensation reaction under alkaline condition, obtaining 2,4,4-Trihydro-xychalcone, (2) subjecting 2,4,4-trihydro-xychalcone and 1-bromo-3-methyl-2-butene to condensation reaction, obtaining 2-hydroxyl-4,4-bis (3-methyl-2-butenyloxy) chalcone, (3) subjecting the 2-hydroxyl-4,4-bis (3-methyl-2-butenyloxy) chalcone and ethyl bromoacetate to condensation under the action of potasium carbonate, thus obtaining sofalcone. The mol ratio of p-hydroxybenzaldehyde, 2.4-dihydroxyacetophenone, 1-bromo-3-methyl-2-butene, and ethyl bromoacetate can be 1 : (0.90-1.50) : (1.60-2.55) : (0.60-1.25).

The invention relates to a method for preparing and separating p-hydroxybenzaldehyde, vanillin and syringaldehyde from lignin, which comprises the following steps: (1) preparing a Lab[1-x]Cu[x]O[3] perovskite type composite oxide catalyst; and (2) carrying out centrifugal separation on a crude aromatic aldehyde product, acidifying, carrying out vacuum drying, and extracting with trichloromethane to obtain a mixture of p-hydroxybenzaldehyde, vanillin and syringaldehyde; dissolving the mixture of p-hydroxybenzaldehyde, vanillin and mixture in anhydrous alcohol, adding ammonia water to form a precipitate, filtering, and regulating the pH value of an alcohol solution of the filtered solid with a sulphuric acid solution, thereby obtaining a crude syringaldehyde product; and concentrating the filtered liquid while depressurizing to obtain a solid, rectifying in a nitrogen atmosphere, and respectively collecting fractions at different temperatures, thereby obtaining the vanillin and p-hydroxybenzaldehyde. The invention increases the comprehensive utilization ratio of the wood fibers, lowers the cost of the wood fiber fuel alcohol, and has great economic and social meanings.

The invention relates to synthesis of a triamine containing a symmetrical triaryl pyridine structure and hyperbranched polyimide thereof. The triamine monomer is BB'2-type aromatic triamine, namely 2,4,6-tris[4-(4-aminophenoxy)-phenyl] pyridine the structure of which is shown in the specification. The triamine is prepared by the following three steps: firstly reacting p-hydroxybenzaldehyde with p-hydroxyacetophenone in acetic acid to obtain 2,4,6-tris(4-hydroxyphenyl) pyridine, then reacting 2,4,6-tris(4-hydroxyphenyl) pyridine with p-chloronitrobenzene to obtain 2,4,6-tris[4-(4-nitrophenoxy)-phenyl] pyridine, and finally reducing the trinitro compound by use of hydrazine hydrate in the presence of a carbon-supported palladium catalyst to synthesize 2,4,6-tris[4-(4-aminophenoxy)-phenyl] pyridine. The hyperbranched polyimide of the triamine is an amino-terminated or anhydride-terminated hyperbranched polyimide polymer obtained by polymerization of the triamine monomer and a commercial dianhydride monomer. The prepared hyperbranched polyimide has excellent high-temperature resistance, solubility and optical properties; and the hyperbranched polyimide polymer material has great application value and prospects in the fields of photosensitive, optical waveguide and gas permeation separation membranes and other materials.

The invention provides a pyrrole di-methine fluorescent dye and a synthesis method and application; the synthesis method is as follows: a. preparing 2-phenylaziridine from styrene; b. adding 2-phenylaziridine into acetophenone, and reacting to produce 2, 4-diphenylpyrrole in the presence of sodium hydride under room temperature; c. adding 2, 4-diphenylpyrrole into p-hydroxybenzaldehyde, then adding chloranil according to the weight proportion 2, 4-diphenylpyrrole : chloranil =1:3-7; reacting under room temperature with stirring, removing excessive chloranil after reaction, and spinning dry to get blue solid pyrromethene; d. adding blue solid pyrromethene into dichloromethane for dissolution, then adding boron trifluoride diethyl etherate under the protection of inert gas, and reacting under room temperature; after reaction, adding chloroform and extracting 2 to 3 times; combining extract liquids, water washing, drying by anhydrous magnesium sulfate, spinning dry, and column separation to yield products.

The invention relates to a preparation method for quizalofop-p-ethyl, in particular to a method which uses p-hydroxybenzaldehyde to replace the raw material hydroquinone used in the traditional technology and react with S (-)-N-tosyl ethyl lactate to prepare R (+)-2-(p-oxy) propionate which is then reacted with 2,6- dichloro-quinoxaline to prepare high-purity quizalofop-p-ethyl through condensation.

The invention provides imidazole [4,5-f]-1,10-phenanthroline derivatives as well as a preparation method and application thereof. The method comprises the following steps: oxidizing 1,10-phenanthroline into 1,10-phenanthroline-5,6-diketone; forming p-hydroxy benzimidazole[4,5-f]phenanthroline with p-hydroxybenzaldehyde in ammonium acetate and glacial acetic acid condition; and forming the imidazole [4,5-f]-1,10-phenanthroline derivatives with 2-dimethylaminoethyl chloride hydrochloride or 1-(2-ethyl) piperidine hydrochloride or 1-(2-ethyl) pyrroline hydrochloride in anhydrous degasified DMF (dimethylformamide) containing NaH. The prepared imidazole [4,5-f]-1,10-phenanthroline derivatives can selectively identify and stabilize telomere G-tetrable helix DNA (deoxyribonucleic acid) in the existence of excessive double helix DNA, and can effectively inhibit growth and propagation of HeLa and HepG2 cancer cells, and can be used for preparing antitumor medicaments.

The invention provides a conductive photo-thermal self-healing composite hydrogel dressing as well as a preparation method and application thereof.The preparation method comprises the following steps:grafting acrylic acid on chitosan to obtain an N-carboxyethyl chitosan polymer; the preparation method comprises the following steps: grafting p-hydroxybenzaldehyde on a triblock copolymer to obtainan aldehyde-terminated polymer (PF127-CHO); the preparation method comprises the following steps: preparing an aldehyde-terminated polymer into a solution, adding carbon nanotubes into the polymer solution, and carrying out ultrasonic treatment in an ice bath to obtain an aldehyde-terminated/carbon nanotube dispersion liquid; the preparation method comprises the following steps: preparing an N-carboxyethyl chitosan polymer into a solution, mixing the solution with an aldehyde group-terminated/carbon nanotube dispersion liquid, and carrying out mutual crosslinking at 20-45 DEG C for 5-400 seconds to obtain the conductive, adhesive, self-healing, photo-thermal and nano composite hydrogel. The hydrogel has excellent adhesion, self-healing, pH response, biocompatibility and hemostatic performance, can show a photo-thermal behavior after being exposed to a near-infrared (NIR) region, causes physical damage to bacteria, and has huge potential for treating infected wounds.

The invention discloses a new process for synthesizing salbutamol. The process comprises the steps that (1) chloromethylation reaction: reactants namely p-hydroxy benzaldehyde and paraformaldehyde react under an acidic condition to generate a compound 1; (2) hydrolysis reaction: the compound 1 is subjected to hydrolysis reaction under a weakly alkaline condition to generate a compound 2; (3) propylidene protective reaction: dihydroxy of a reactant 2 is subjected to propylidene protection under catalysis of concentrated sulfuric acid; (4) epoxidation reaction: a reactant 3 reacts to obtain a compound 4 by using the effect of strong base under the effects of a ylide reagent and a phase transfer catalyst; (5) aminolysis ring-opening reaction: the compound 4 is heated and refluxed in tert-butylamine, and is subjected to aminolysis ring-opening reaction to obtain a compound 5; (6) hydrolysis de-protective reaction: the compound 5 is subjected to hydrolysis reaction under the acidic condition to obtain salbutamol. The new process disclosed by the invention is mild in reaction condition, easy in purification, and simple and easily-available in raw materials; the total molar yield of the process reaches up to 45%, and the product quality reaches up to more than 99.5%.

The present invention provides an epoxy resin toughening agent based on cyclotriphosphazene six-arm star polymer and a preparation method for the epoxy resin toughening agent, and belongs to the technical field of epoxy resin modification. The preparation method for the toughening agent comprises the following steps of: step I, in the presence of an acid scavenger, generating a nucleophilic substitution reaction in an oargnic solvent by utilizing hexachlorocyclotriphosphazene and p-hydroxybenzaldehyde, and obtaining a solid after separation and drying; step II, in the presence of a reductant, reducing a solid aldehyde group obtained in the step I to a hydroxyl group; and step III, by taking the solid obtained in the step II as an initiator, initiating ring-opening polymerization of caprolactone and obtaining the toughening agent after separation and drying. The epoxy resin toughening agent based on cyclotriphosphazene six-arm star polymer provided by the present invention has significant toughening effect on epoxy resin and can significantly improve impact resistance of the epoxy resin without sacrificing other mechanical properties and thermal properties of the material, thereby facilitating industrialized production.

The invention discloses a preparation method of six-functionality epoxy resin based on cyclotriphosphazene, which aims at solving the technical problem of poor comprehensive property in the existing prepared epoxy resin flame-retardant system. The preparation method adopts the technical scheme with the following steps of firstly, performing nucleophilic substitution on p-hydroxybenzaldehyde and phosphonitrilic chloride trimer under the condition of alkaline existence, so as to obtain a hexaaldehyde compound HAPCP; using sodium borohydride or lithium borohydride to reduce the HAPCP, so as to obtain a hexahydroxy intermediate HHPCP; dissolving the HHPCP, bromopropylene and alkaline into an organic solvent, so as to obtain HAMPCP; oxidizing a hexaalkenyl-containing compound HAMPCM by metachloroperbenzoic acid in an organic solvent, so as to obtain a hexaepoxy target product HGPCP. The preparation method has the advantages that because the molecular structure of HGPCP contains six epoxy functional groups, the mechanical property and heat-resistant property are improved; by containing the cyclotriphosphazene structure with the flame-retardant property, the flame-retardant property is very excellent, the limited oxygen index is greater than 30%, and the UL-94 reaches V-0 level.

The present invention relates to process of preparing 4, 4'-diamido-4''-hydroxy triphenyl methane. The process includes the following steps: 1. reaction of aniline and hydrochloric acid solution in the molar ratio of 1.0 to 1.0-1.5 at room temperature for 0.1-4 hr, adding water insoluble organic solvent, heating reflux to separate out water, cooling, filtering and drying to obtain aniline hydrochloride; and 2. reaction of p-hydroxybenzaldehyde and aniline in the molar ratio of 1.0 to 2.0-4.0 in nitrogen with aniline hydrochloride as catalyst at 80-120 for 1-8 hr, cooling, vacuumizing, eliminating excessive aniline, adding alcohol solvent, heating to dissolve, cooling to crystallize, filtering and drying to obtain purple needle-shaped 4, 4'-diamido-4''-hydroxy triphenyl methane crystal. The present invention has simple operation, low cost and high product purity, and is suitable for industrial production.

The invention discloses a preparation method and application of a mitochondrion-targeted double-signal turn-on formaldehyde fluorescent nano probe intermediate compound (V). The method comprises the following steps: activating p-hydroxybenzaldehyde used as an initial raw material in the presence of an acid-binding agent at 60-70 DEG C, and performing a nucleophilic substitution reaction in an acetone solvent by using 3-bromopropyne as a nucleophilic reagent to obtain a compound (II); performing ammonification on the compound (II) at 0 DEG C by means of an ammonia methanol solution, adding allylboronic acid pinacol ester, performing mixing, and performing a reaction while the temperature is controlled at 25-35 DEG C to obtain a compound (III); and performing a Schiff base reaction on 3-formyl-4-hydroxyl-1,8-naphthalimide and the compound (III) under the action of Lewis acid and a reducer, and performing a reduction reaction to obtain the compound (V). The compound (V) can be used as theintermediate compound for preparing a double-signal turn-on formaldehyde fluorescent nano probe. The nano probe reacts with formaldehyde to obtain two free fluorescent substances, thereby achieving adouble turn-on effect, and improving the detection accuracy. The compound (II), the compound (III) and the compound (V) are as shown in the specification.

The invention provides a coumarin derivative DOCOPA as well as a preparation method and an application thereof. The English name of DOCOPA is (E)-4-(3-(7-(diethylamino)-2-oxo-2Hchromen-3-yl)-3-oxoprop-1-en-1-yl) phenylacrylate). The preparation method comprises the steps that 3-acetyl-7-diethylaminocoumarin and p-hydroxybenzaldehyde are dissolved in acetonitrile firstly, a catalytic amount of piperidine is added, and reflux is performed until a reaction is performed sufficiently; an intermediate compound is further obtained; the intermediate compound and triethylamine are dissolved in dichloromethane, acryloyl chloride is added dropwise gradually to an ice bath, room-temperature stirring is performed until a reaction is performed sufficiently, a product is subjected to column chromatography separation after reduced-pressure evaporation, and the DOCOPA is obtained. The DOCOPA is applied to distinguishing and detection of cysteine and homocysteine in a pH7.8 system and imaging of the cysteine and the homocysteine in cells. The DOCOPA shows high sensitivity and selectivity for the cysteine and the homocysteine.

The invention discloses a 2,4,6-diethyl triphosphate hydroxymethylphenoxyl-1,3,5-triazine flame retardant and a preparation method thereof and belongs to the technical field of flame retarding. The preparation method comprises following steps: 1) adding cyanuric chloride, p-hydroxybenzaldehyde and a catalyst to an organic solvent, performing a heat reflux reaction and performing after-treatment to obtain a white solid powder 2,4,6-trialdehydephenoxyl-1,3,5-triazine; and 2) adding the 2,4,6-trialdehydephenoxyl-1,3,5-triazine, diethyl phosphite and triethylamine to an organic solvent, performing a heat reflux reaction, and performing pressure-reduced distillation to a reaction product to remove the organic solvent and the triethylamine to obtain the 2,4,6-diethyl triphosphate hydroxymethylphenoxyl-1,3,5-triazine flame retardant. The flame retardant is simple in preparation method, is high in yield, is good in practicability, is environment-friendly and pollution-free, and is available in large-scale industrial production.

The invention discloses a cyclophosphazene compound and synthesizing method as photographic flame-proof material, which comprises the following parts: cyclophosphazene, p-hydroxybenzoic acid, potassium acrylate, potassium methyl acrylate, acryloyl chloride or methyl acryloyl chloride.

The invention provides a brand new preparation method of ciprofibrate. The method is characterized in that the method comprises the following steps: decarboxylating cheap and easily-available p-hydroxybenzaldehyde as a raw material, carrying out hydroxy group protection, cyclizing, deprotecting, and carrying out a Bargellini reaction to prepare ciprofibrate. Compared with traditional methods, the method provided by the invention has the advantages of simple operation, mild and easily-controlled conditions, post-treatment convenience, environmental protection and high yield, has a high safety because of the avoiding of the use of a large amount of peroxy acid or hydrogen peroxide, and is a brand new environmentally-friendly method suitable for the industrial synthesis of ciprofibrate.

The invention discloses a method for synthesizing (R)-salmeterol. The method is implemented by taking p-hydroxy benzaldehyde as a raw material through the steps of carrying out a methylolation reaction on the p-hydroxy benzaldehyde so as to obtain prochiral aldehyde for protecting double hydroxide radicals in an acetal form; then, through taking (S)-BINOLAM.AlCl as a chiral catalyst, carrying out an asymmetric nucleophilic addition reaction so as to obtain a chiral cyanohydrin intermediate; and reducing the chiral cyanohydrin intermediate so as to obtain primary amine, reacting the primary amine with mesylate [6-(4 phenylbutoxy]hexane, and carrying out hydrolysis on the obtain product so as to remove protecting groups, thereby obtaining a final product (R)-salmeterol. In the invention, a chiral catalyst precursor (S)-BINOLAM can be reused; and the method has relatively high yield and relatively good enantioselectivity, and is short in synthetic route, simple and convenient in operation and low in cost.

The invention discloses a preparation method of highly-pure benzyl aryl ether 4-(3-fluorobenzyloxy)-benzaldehyde and a derivative thereof. The method is characterized in that the benzyl aryl ether 4-(3-fluorobenzyloxy)-benzaldehyde and the derivative thereof are prepared through condensation of a benzyl derivative and p-hydroxybenzaldehyde in the presence of an organic alkali. The method has the characteristics of mild reaction conditions, simplicity in operation, good reaction selectivity, high product purity, and easy realization of industrial production.

The invention discloses a synthesis method of p-hydroxy-beta-nitrostyrene, which comprises the following step: synthesizing p-hydroxybenzaldehyde and nitromethane used as raw materials into p-hydroxy-beta-nitrostyrene by using ammonium acetate as a catalyst and glacial acetic acid as a solvent, wherein an antioxidant anhydrous hydroquinone is added to protect the raw material p-hydroxybenzaldehyde from oxidation, and toluene is added in the later reaction period to take the generated water out of the reaction system, so that the reaction proceeds in the positive reaction direction. The method has the advantages of low reaction cost, high product yield, simple after-treatment and the like, and the yield of the hydroxy-beta-nitrostyrene can reach higher than 92%.