36 results about "Methyl-p-benzoquinone" patented technology

Process for the preparation of 2,3,5-trimethyl-p-benzoquinone by oxidizing 2,3,5-trimethylphenol or 2,3,6-trimethylphenol with oxygen or an oxygen-containing gas mixture in the presence of a catalyst system which can be a copper halide and a transition metal halide; for example iron, chromium, manganese, cobalt, nickel, zinc or a rare earth halide, in a two-phase reaction medium, at elevated temperature.

The invention discloses a method for preparing 2,3,5-trimethylhydroquinone, which comprises oxidizing 2,3,6-trimethylphenol with pure oxygen or oxygen-enriched gas in water serving as a reaction medium in the presence of a catalyst consisting of copper halide and lithium halide and a phase transfer catalyst to obtain 2,3,5-trimethylhydroquinone. In the method disclosed by the invention, organic solvent is not added, the production safety is ensured, the operation is simplified, the energy cost is greatly reduced, the yield of the obtained product is over 90 percent, and the purity of the obtained product is over 99.5 percent. Thus, the method is suitable for industrial mass production.

The invention relates to a double-enzyme one-pot synthesis method of 2,3-dimethyl-5alkylamino-1,4-benzoquinone. By the utilization of a crosslinked laccase / lipase aggregation system for catalyzing phenol oxidation / C-N cross-coupling cascade reaction, 2,3-dimethyl-5alkylamino-1,4-benzoquinone is prepared. laccase catalyzes 2,3-dimethylhydroquinone oxidation to generate 2,3-dimethyl-p-benzoquinone,and lipase catalyzes 2,3-dimethyl-p-benzoquinone and fatty primary amines for the C-N cross-coupling reaction so as to prepare the product. The yield reaches 95% and above. According to the technologyfor concerted catalysis of phenol oxidation / C-N cross-coupling reaction by the utilization of lipase and laccase, yield of the product is raised by about 200% in comparison with single laccase catalysis; and the method has higher selectivity than a traditional chemocatalysis method, and by-products are less. The method of the invention is a green and environmentally-friendly synthesis method.

The present invention discloses a method for synthesizing a benzoquinone compound through catalytic oxidation of a phenol compound, and belongs to the technical field of synthesis of benzoquinone compounds. The method comprises: adding a reactant phenol compound, a solvent, a solid catalyst (onion carbon and the like) and an oxidant t-butyl hydroperoxide into a reactor, carrying out ultrasonic treatment to form a suspension, heating the suspension to a temperature of 70-100 DEG C, carrying out a reaction for 2-16 h, separating the reaction mixture to obtain a solid catalyst and a liquid mixture containing the benzoquinone compound, and carrying out separation purification on the liquid mixture to obtain the product benzoquinone compound. According to the present invention, the operation process is simple, and the used non-metal catalyst has characteristics of no corrosion, low price, green environmental protection and recycling; and the methyl phenol conversion rate is high, and the selectivity of the target product methyl-p-benzoquinone is good.

The invention provides a carbon nanotube-based sensing material. The sensing material comprises a single-walled carbon nanotube and 2, 3, 5, 6-tetrafluoro-7, 7', 8, 8'-tetracyanoquinodimethan, wherein2, 3, 5, 6-tetrafluoro-7, 7', 8, 8'-tetracyanoquinodimethan is adsorbed on the surface of the single-walled carbon nanotube through non-covalent interaction. The invention further provides a preparation method of the sensing material and an application of the sensing material in organic amine volatile gas detection. Based on the strong electron-absorption effect of a plurality of electron-withdrawing functional groups of the 2, 3, 5, 6-tetrafluoro-7, 7', 8, 8'-tetracyanoquinodimethan, a strong non-covalent interaction is formed with the carbon nanotube, so that the sensitivity of the sensingmaterial to the organic amine volatile gas is increased.

The decompression gas stripping process is used for aniline or o-toluamide oxidizing process to produce p-benzoquione, o-methyl-p-benzoquione and quinol or o-methyl quinol in a closed production system in the pressure of 50mmHg-750mmHg, stripping tower top temperature of 40 deg.c-100 deg.c, condenser pipe temperature of 20 deg.c-100 deg.c and crystallizing tank or reducing pot temperature of 15 deg.c-100 deg.c. Compared with conventional process, the present invention has 6-15 % raised product yield.

The invention discloses a copper-7, 7, 8, 8-tetracyanoquinodimethane material and a preparation method and an application thereof. The method comprises the following steps: in an inert atmosphere, dissolving -7, 7, 8, 8-tetracyanoquinodimethane in acetonitrile; and then, adding cuprous iodide, and carrying out a reaction under reflux to obtain the material. The material prepared by the invention can be used for preparing organic thermoelectric materials. Through verification, the thermoelectricity of the copper-7, 7, 8, 8-tetracyanoquinodimethane doped by 2, 3, 5, 6-tetrafloro-7, 7', 8, 8'-tetracyanodimethyl p-benzoquinone is remarkably improved, for instance, when the dosage concentration of 2, 3, 5, 6-tetrafloro-7, 7', 8, 8'-tetracyanodimethyl p-benzoquinone under 360K is 1mol%, the power factor is improved from 1.4 mu W / mK<2> to 2.2 mu W / mK<2>. Meanwhile, the preparation method provided by the invention is simple in process, easy in preparation and low in cost.

The invention discloses a catalyst suitable for catalytic oxidation of 2,3,6-trimethylphenol for preparing 2,3,5-trimethyl p-benzoquinone, and belongs to the technical field of preparation of catalysts. The catalyst is prepared from Co(Salphen) and a bipyridine compound; the bipyridine compound comprises two contrapuntal pyridyls, and a Co atom in the Co(Salphen) and a nitrogen atom in the bipyridine compound are connected with each other by a coordination bond, so as to form a non-covalent polymer catalyst. The catalyst is simple in preparation method, the 2,3,5-trimethyl p-benzoquinone can be generated through catalytic oxidation of the 2,3,6-trimethylphenol by taking O2 as an oxidizing agent at room temperature and normal pressure, the limit that most of the type of heterogeneous reactions need hydrogen peroxide and high temperature before is overcome, and the conversion rate of a substrate and the selectivity of a product in a recycling process of the catalyst can be well maintained.

The invention discloses 2, 3, 5, 6-tetrafluoro-7, 7', 8, 8'-tetracyanoquinodimethane and a preparation method thereof. The preparation method comprises diazotization: carrying out diazotization of a compound A and a compound B to obtain a compound C, reduction: reducing the compound C into a compound D, oxidation: oxidizing the compound D into a compound E, and condensation: condensing the compound E and malononitrile to obtain a compound F, wherein the compound F is 2, 3, 5, 6-tetrafluoro-7, 7', 8, 8'-tetracyanoquinodimethane and the compounds A, B, C, D, E and F are shown in the description. The preparation method has good environmental friendliness and a high yield of 80% or more, is simple and easy and is suitable for industrial production.

The invention relates to a medicinal composition for inhibiting angiogenesis and application thereof. The medicinal composition comprises any one composition of 2-methoxy-6-methyl-P-benzoquinone(2-methoxy-6-methyl-p-benzoquinone), 2,3-dimethoxy-5-methyl-P-benzoquinone(2,3-dimethoxy-5-methyl-p-benzoquinone) or 2-hydroxy-5-methoxy-3-methyl-P-benzoquinone(2-hydroxy-5-methoxy-3-methyl-p-benzoquinone) and appropriate pharmaceutically acceptable excipients or supporting agents; and the medicinal composition is used for inhibiting the angiogenesis and further treats or prevents angiogenesis-related diseases.

The invention relates to a process for preparing 2,3,5-trimethyl p-benzoquinone by means of catalytic oxidation, belonging to the technical field of preparation of the 2,3,5-trimethyl p-benzoquinone.A new process for preparing the 2,3,5-trimethyl-p-benzoquinone is formed by combining a supergravity reactor with the conventional stirred tank reactor. The process uses pure-oxygen or oxygen-rich gasas an oxidant and takes an aqueous solution of a metal halide as a catalyst, a reactant, i.e., 2,3,6-trimethylphenol is dissolved in an organic solvent, and the whole reaction process is carried outin the supergravity reactor and the stirred tank reactor. The supergravity reactor has an ability to enhance liquid-liquid mixing and gas-liquid mass transfer, so that the process can enhance the catalytic effect of the catalyst, increase the reaction rate and shorten the production time; in addition, due to the introduction of the supergravity reactor, the utilization rate of oxygen is increased,an oxidation reaction of the 2,3,6-trimethylphenol is promoted, and the yield of the product per unit time is increased.

The invention relates to a method for detecting diethyl chlorophosphate gas and / or sarin toxic gas based on a charge transfer complex. The method comprises the steps that a first compound containing aN,N dimethyl aromatic amine structure and a second compound containing a tetracyanoquinodimethane structure interacts through intermolecular charge transfer in a solvent to obtain a solution of the charge transfer complex; a sensing material is loaded on the surface of an electrode to form a sensor piece; and the sensor piece is put into the atmosphere containing the diethyl chlorophosphate gas and / or the sarin toxic gas to be detected. According to the method, through the charge transfer complex formed by mixing of the first compound and the second compound in the solvent, the high electronmobility and high hole mobility are achieved, the independent chemical physical properties of the first compound and the second compound are maintained while complexing is conducted, the charge transfer complex can serves as an electrochemical sensing probe to detect the sarin toxic gas, and the problems that in the prior art, detection sensitivity of the sarin toxic gas is low, specificity is low, the means is complex, and the cost is high are solved.

The invention discloses a device capable of producing a photoelectric effect and electroluminescence simultaneously and a preparation method thereof. The photoelectric device is acquired through packaging a cadmium sulfide / cadmium telluride heterogeneous junction nano-rod, and specifically comprises an anisotropic conductive film, an Al electrode, ZnO, a heterogeneous junction nano-rod, 2, 3, 5, 6-tetrafluoro-7, 7', 8, 8'-tetracyanoquinodimethane, TCNQF4 and the like. The invention further discloses a preparation method of the photoelectric device.

The invention discloses a method for producing o-methyl hydroquinone from o-methyl p-benzoquinone through reduction of a sulfur series reducing agent. The method comprises the following steps: addingwater in an o-methyl-p-benzoquinone extracting solution, introducing in the sulfur series reducing agent, stirring for reacting, and sampling and analyzing until no o-methyl-p-benzoquinone exists in asystem, i.e., reaching a reaction endpoint; standing the solution, and extracting, thus obtaining an o-methyl hydroquinone extracting solution; extracting a mixed solution generated through reductionreaction, thus obtaining an extracting solution; adding water in the extracting solution, and removing an extracting agent by carrying out decompression and desolventization, thus obtaining an o-methyl hydroquinone water solution; then carrying out decoloration, vacuum concentration, cooling and crystallizing, and drying, thus obtaining an o-methyl hydroquinone product. Compared with a traditional iron powder reduction technology, the method disclosed by the invention is moderate in reaction conditions, is efficient and energy-saving, is clean and environmentally friendly and has high conversion rate and good product quality; meanwhile, compared with palladium carbon catalytic hydrogenation, the method is short in reaction time, low in input cost and small in product loss, a reaction product-sulfuric acid can be used as a raw material for preparing o-methyl p-benzoquinone through an aniline method, and the method is more economic.

The invention discloses a device capable of simultaneously generating the photoelectric effect and electroluminescence and a making method thereof. The material is acquired through packaging heterojunction nano rods, specifically, an anisotropy conductive film, an Al electrode, ZnO, the heterojunction nano rods, 7,7',8,8'-tetrafluoro 2,3,5,6-tetracyano- p-quinodimethane and TCNQF4 are included. The invention further discloses a making method of the device.

The invention provides a method for synthesizing targeted antioxidant SKQ1 intermediate 2,3-dimethyl-p-benzoquinone, comprising the following steps: 1) 2,3-dibromo-5,6-dimethyl- P-benzoquinone was dissolved in glacial acetic acid, added reduced iron powder, stirred at room temperature for 1 hour, then heated and refluxed for 5 hours; 2) After cooling, the reaction mixture was filtered and the solvent in the filtrate was evaporated under reduced pressure, and the recovered glacial acetic acid could be Recycle and reuse, the crude product is dissolved in ethanol and adjusted to pH 9 with 5% aqueous sodium hydroxide solution, and air flow is introduced until the mixture becomes dark blue, and the reaction is completed by TLC monitoring; 3) The reaction mixture is acidified with 10% HCl To pH 4, most of the ethanol was evaporated under reduced pressure, then extracted three times with ethyl acetate, the organic phases were combined, the solvent was spin-dried to obtain an oily crude product, ethyl acetate was recovered, and the crude product was purified by silica gel flash column to obtain a pale yellow oily product. The invention synthesizes a mitochondrial antioxidant SKQ-1 intermediate, 2,3-dimethyl-p-benzoquinone; the solvent can be reused repeatedly, and the production cost is saved; it provides a raw material basis for industrialized synthesis of the mitochondrial antioxidant SKQ1.

The invention discloses a method for preparing methylbutylamine p-benzoquinone through lipase catalysis. The method is characterized by comprising a step of catalyzing butyl amine to react with methylp-benzoquinone by using immobilized candida antarctica lipase, thereby obtaining 2-methyl-5-methylbutylamine p-benzoquinone. The 2-methyl-5-methylbutylamine p-benzoquinone is prepared by using an enzyme catalysis method, because of high spatial selectivity of an enzyme, difficulties that a chemical synthesis process is poor in selectivity and hard in product separation can be avoided, and the method is an environmental-friendly efficient synthesis method.

The present invention provides a synthetic method of targeted antioxidant SKQ1 intermediate 2,3-dibromo-5,6-dimethyl-p-benzoquinone, comprising the following steps: 1) converting 2,3-dimethylphenol Dissolve in methanol, add bromine dropwise at 0°C, slowly rise to room temperature and stir for 2 hours; 2) Cool the reaction solution to 0°C, add 30% hydrogen peroxide aqueous solution dropwise, the reaction is exothermic, and the reaction temperature is controlled Below 30°C, after the dropwise addition, rise to room temperature and react overnight; 3) Drain the solvent under reduced pressure, recover methanol (it can be reused after simple drying), add ethyl acetate to dissolve the oily crude product, and dissolve it with 10% carbonic acid Washing with sodium hydrogen; 4) Drain the solvent of the crude ethyl acetate solution in step 3), the recovered ethyl acetate can be recycled, and the oily crude product is purified with a silica gel column to obtain a light green pure product powder. The present invention synthesizes a novel SKQ-1 intermediate 2,3-dibromo-5,6-dimethyl-p-benzoquinone; the solvent can be reused to save production costs; it is a new route to synthesize mitochondrial antioxidant SKQ1 Provide raw material basis.

The invention discloses a catalyst suitable for catalytic oxidation of 2,3,6-trimethylphenol for preparing 2,3,5-trimethyl p-benzoquinone, and belongs to the technical field of preparation of catalysts. The catalyst is prepared from Co(Salphen) and a bipyridine compound; the bipyridine compound comprises two contrapuntal pyridyls, and a Co atom in the Co(Salphen) and a nitrogen atom in the bipyridine compound are connected with each other by a coordination bond, so as to form a non-covalent polymer catalyst. The catalyst is simple in preparation method, the 2,3,5-trimethyl p-benzoquinone can be generated through catalytic oxidation of the 2,3,6-trimethylphenol by taking O2 as an oxidizing agent at room temperature and normal pressure, the limit that most of the type of heterogeneous reactions need hydrogen peroxide and high temperature before is overcome, and the conversion rate of a substrate and the selectivity of a product in a recycling process of the catalyst can be well maintained.

The invention relates to the field of material preparation, in particular to a photo-thermal conversion eutectic material containing pyrene and a preparation method of the photo-thermal conversion eutectic material. The eutectic material formed by PY and tetracyanoethylene (TCNE) as well as 7, 7, 8, 8,-tetracyanodimethyl p-benzoquinone (TCNQ) has excellent photo-thermal conversion performance, and particularly, the photo-thermal conversion efficiency in a near-infrared region is very high. Besides, the eutectic material has excellent photo-thermal conversion performance and high thermal stability, the preparation conditions are mild and simple, the cost is low, and the two materials belong to two new materials and are particularly related to photo-thermal conversion, sewage treatment, seawater desalination, photo-thermal imaging and photo-thermal treatment.

The invention discloses a P-type doping method for a semiconductor layer of an organic field effect transistor and the prepared organic field effect transistor, and the method comprises the steps: dissolving 2, 3, 5, 6-tetrafluoro-7, 7 ', 8, 8'-tetracyanodimethyl p-benzoquinone (F4-TCNQ) in an orthogonal solvent of the organic semiconductor layer to serve as a P-type doping agent; the method comprises the following steps of: preparing an organic semiconductor layer film, spin-coating the organic semiconductor layer film on the spin-coated organic semiconductor layer film in an air atmosphere, and activating doping through rapid thermal annealing, so that the problems caused by jump transmission and coulomb traps in charge transport are solved, the threshold voltage is reduced, and the switch ratio is increased. For the P-type field effect transistor, the P-type doping enhances the hole transport, effectively improves the saturation current, and inhibits the electron transport, so that the power consumption is reduced when the transistor is closed. The doping method is operated based on a solution method, is simple in process and low in preparation cost, can be suitable for large-scale production, and has a very good prospect in application of flexible and portable electronic equipment.