355 results about "Malonic acid" patented technology

The invention belongs to the field of precious metal recovery, and particularly relates to a method for leaching silver from a silver-containing retired crystalline silicon solar cell. According to the method, the silver in the silver-containing decommissioned crystalline silicon solar cell is recycled and leached through the synergistic effect of an HNO3-H2O2-Fe < 3 + > composite leaching agent and ionic liquid, and the ionic liquid is prepared from choline chloride and malonic acid. Meanwhile, the leaching rate of silver is further improved by optimizing experimental parameters such as the reaction temperature, the reaction time and the H2O2 supply frequency in the three-section gradient temperature control leaching reaction. Compared with the traditional technology, the method disclosed by the invention is green and environment-friendly, low in cost, small in acid consumption and high in recovery rate.

The invention belongs to the technical field of separation of drug intermediates, and particularly relates to a control method for a process impurity 2-ethyl valeric acid (EP-B) in preparation of valproic acid or sodium valproate by a diethyl malonate method. According to the method disclosed by the invention, the content of 2-ethyl-2-propylmalonic acid process impurities in dipropylmalonic acid is controlled, so that the content of 2-ethylvaleric acid (EP-B) which is a process impurity in valproic acid or sodium valproate is accurately controlled; adding a polar solvent into the dipropylmalonic acid crude product, heating, pulping for a certain time, cooling, filtering and drying to obtain a high-purity dipropylmalonic acid refined product; high-purity valproic acid (RRT is equal to 1.00) is prepared through decarboxylation of the dipropyl malonic acid fine product, and the purity is 99.779%; 0.020% of 2-ethyl valeric acid (RRT is equal to 0.90); and valeric acid (RRT = 0.77), 0.039%. The valproic acid product quality meets the requirements of European Pharmacopoeia. According to the method, the problems of quality control and process evaluation of valproic acid or sodium valproate prepared by a diethyl malonate method are solved.

The present invention relates to a preparation method and application of a supramolecular aggregate surfactant, and belongs to the field of supramolecular coordination chemistry, surface modification engineering and hydrophobic coating technology. In the present invention, 4-hydroxypyridine-2,6-dicarboxylic acid and malonic acid prepare an adhesive ligand, and with the help of the coordination of the carboxyl structure and lanthanum ions on 4-hydroxypyridine-2,6-dicarboxylic acid and perfluorooctanoic acid, a supramolecular aggregate in a nano-aggregated state is obtained, which is self-assembled into a supramolecular aggregate surfactant. The active agent can solubilize fluoride and can also be applied in the field of hydrophobic coatings. The coating has the characteristics of imitating lotus leaf structure and hydrophobic wax, and has good hydrophobic properties.

The invention relates to the technical field of biological extraction, in particular to a preparation method of selenium polysaccharide in cardamine violifolia, which comprises the following steps: extracting selenium polysaccharide in cardamine violifolia by using a deep eutectic solvent as an extraction solvent and adopting an ultrasonic method, and removing protein in the selenium polysaccharide by using an isoelectric precipitation method and an enzymolysis method, thereby obtaining the selenium polysaccharide in cardamine violifolia. Removing water, enzymolysis product amino acid, inorganic selenium and other impurities by a membrane separation concentration system to obtain cardamine violifolia selenium polysaccharide; wherein the eutectic solvent comprises choline chloride and malonic acid in a molar ratio of 1: 1-1: 3, and the water content is 40-60% (mass percent); the compound enzyme is prepared from bromelain and papain in a mass ratio of 1: 1. Protein in the selenium polysaccharide is removed by adopting deep eutectic solvent ultrasonic extraction and an isoelectric precipitation method combined with an enzymolysis method, enzymolysis product amino acid, inorganic selenium and other impurities are removed by adopting an ultrafiltration membrane separation and concentration system, the structure of the polysaccharide is not damaged, and the high-purity cardamine violifolia selenium polysaccharide is obtained.

The invention belongs to the technical field of separation of drug intermediates, and particularly relates to a method for preparing a high-purity dipropylmalonic acid refined product by adding a polar solvent into a dipropylmalonic acid crude product, heating, pulping for a certain time, cooling, filtering and drying. Decarboxylating the refined dipropylmalonic acid product to obtain high-purity valproic acid; distilling the filtrate to recover the polar solvent to obtain 2-methyl-2-propylmalonic acid, and carrying out decarboxylation on the 2-methyl-2-propylmalonic acid to obtain 2-methylpentanoic acid; 2-methylvaleric acid is used as a perfume additive. According to the method disclosed by the invention, the process impurity 2-methyl-2-propylmalonic acid in dipropylmalonic acid is separated, and the process impurity 2-methylvaleric acid (EP-L) in valproic acid or sodium valproate is precisely separated; the quality of the valproic acid product prepared by the method disclosed by the invention meets the requirements of European Pharmacopoeia EP-11 (2023). According to the invention, the problems of quality control and process evaluation of valproic acid or sodium valproate prepared by a dimethyl malonate method are solved.

The invention discloses a synthesis process of chiral cyclic ether indole. The synthesis process comprises the following steps: reacting 4-bromobenzaldehyde with malonic acid under the catalysis of piperidine to generate olefin carboxylic acid CHP-1; carrying out condensation reaction to prepare CHP-2; under the catalysis of a copper reagent, carrying out Michael addition reaction to obtain CHP-3; preparing a chiral alcohol intermediate CHP-4 through a reduction reaction; trifluoromethanesulfonic acid is used, and a chiral ether intermediate CHP-5 is prepared through ring closing; reacting with protected hydrazine by using a copper ion catalyst to obtain an intermediate CHP-6; the method comprises the following steps: by taking alcohol as a solvent, adding strong acid, and removing a protecting group of hydrazine to obtain an intermediate CHP-7; and carrying out ring closing by taking lewis acid as a catalyst to obtain an indole product CHP-8. The use of a noble metal catalyst palladium is avoided, and the cost is greatly reduced. The chiral center is directly constructed through a chemical method, and SFC is not needed for resolution, so that the cost is remarkably reduced, and industrial production is successfully realized.

The invention discloses an improved self-induction culture medium and a culture process, and belongs to the technical field of bioengineering. The improved self-induction culture medium is prepared from 10 g / L of glucose, 3-5 g / L of glycerin, 3 g / L of lactose, 24 g / L of yeast extract, 8 g / L of casein hydrolysate, 0.02-0.05 mM of malonic acid, 1 mM of methionine and 1-3 mM of MgSO4, a phosphate buffer solution is added to control the pH to be 7.2, and the improved self-induction culture medium is prepared by mixing after sterilization. Cells are inoculated to an improved self-induction culture medium for culture, automatic switching of growth-induction stages can be realized based on a pH and DO linkage dynamic feeding control method, the operation complexity is reduced, and the controllability is higher. The culture medium does not need a special inducer, cost is reduced, and protein expression quantity is improved.

The invention discloses a synthesis method of 5-bromoindole-2-carboxylic acid methyl ester, and the synthesis route comprises the following steps: S1, taking 2-iodo-4-broronitrobenzene and dimethyl malonate as raw materials, and under the catalysis of a solid sulfonic acid resin catalyst, carrying out nucleophilic substitution reaction to prepare 2-(5-bromo-2-nitrophenyl) dimethyl malonate; s2, taking the dimethyl 2-(5-bromo-2-nitrophenyl) malonate prepared in the step S1 as a raw material, taking a ZSM-5 molecular sieve loaded with cobalt acetate as a catalyst, and introducing hydrogen for reduction reaction to prepare a 5-bromoindole-2-carboxylic acid methyl ester crude product; and S3, carrying out recrystallization on the 5-bromoindole-2-carboxylic acid methyl ester crude product prepared in the step S3 by using ethanol, so as to prepare a 5-bromoindole-2-carboxylic acid methyl ester pure product. The synthesis yield is relatively high, the environmental protection property is relatively good, and the prepared 5-bromoindole-2-carboxylic acid methyl ester is relatively excellent in quality and relatively low in cost.

The invention discloses a low-temperature cured polyurethane varnish resin for automobiles and a preparation method thereof, and belongs to the technical field of chemical product processing, the low-temperature cured polyurethane varnish resin comprises a resin matrix and a curing agent, the resin matrix comprises a component A and a component B. The component A comprises a crosslinking system A1, a crosslinking system A2 and an auxiliary agent, the component B is a curing activity regulator of a double-crosslinking system of the crosslinking system A1 and the crosslinking system A2; the curing agent is diethyl malonate blocked isocyanate; the cross-linking system A1 is mainly composed of hydroxy acrylic resin containing beta-diketone metal ligand and a bismuth neodecanoate catalyst; the bismuth neodecanoate catalyst and a beta-diketone metal ligand form a bismuth complex; the cross-linking system A2 is mainly composed of hydroxyl acrylic resin containing alkoxy silane groups; the component B is prepared from poly (decane-4, 6-diyne diacid) modified nano porous fibers and a silane coupling agent. The service life of the varnish is prolonged on the basis of ensuring low-temperature rapid curing.

The invention belongs to the technical field of fine chemical engineering, and discloses a synthesis method of a malonate compound, which comprises the following steps: under the action of a heterogeneous catalyst, carrying out hydrolysis-esterification reaction on cyanoacetic acid and alcohol, and after the reaction is finished, carrying out post-treatment to obtain the malonate compound, the heterogeneous catalyst comprises a carrier and an active component; the active component comprises ionic liquid and active metal; the carrier is an ordered mesoporous material; the active metal is alkaline earth metal. According to the method, malonate products can be obtained, the problems of low yield, serious equipment corrosion and large amount of three wastes are solved, efficient synthesis of malonate compounds is realized, meanwhile, the production efficiency is improved, and the environmental pollution is greatly reduced.

The invention discloses a solid electrolyte, a secondary battery and an electric device, and belongs to the technical field of batteries, the solid electrolyte comprises a polymer solid electrolyte, a lithium salt and a cross-linked copolymer; the cross-linked copolymer comprises a polymer solid electrolyte containing a carbon-carbon double bond and bis (10-undecylene-1-yl) malonate grafted fullerene. The solid electrolyte can effectively improve the transference number of lithium ions, improve the mechanical property of the solid electrolyte and effectively prolong the cycle life of a secondary battery.

The invention relates to the field of road asphalt, and discloses high-modulus modified asphalt for improving road performance and a preparation method thereof, the modified asphalt comprises matrix asphalt, coal liquefied asphalt, modified rubber seed oil, ethylene-vinyl acetate copolymer and modified carbon nanotubes; the modified rubber seed oil is prepared from epoxy rubber seed oil and a carboxylated flame-retardant component prepared by reaction of amino trimethylphosphonic acid, trimethylolpropane and malonic acid; the modified carbon nano tube is prepared from a toluene-2, 4-diisocyanate isocyanated carbon nano tube and an aminated modifier through a reaction; the amination modifier is prepared by performing acylating chlorination grafting on 3-(3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid by using thionyl chloride and then grafting with p-phenylenediamine. According to the invention, the coal liquefaction asphalt, the modified rubber seed oil, the ethylene-vinyl acetate copolymer and the modified carbon nanotube are added into the matrix asphalt; the high and low temperature performance, the flame retardant performance and the anti-aging performance of the asphalt material can be improved.

The invention relates to a Cu3Ni / NF nanosheet self-supporting electrode and a preparation method thereof, and belongs to the technical field of electro-catalysis. The preparation method of the Cu3Ni / NF nanosheet self-supporting electrode comprises the following steps: mixing CuCl2. 2H2O, polyethylene glycol and malonic acid, heating and stirring to obtain a deep eutectic solvent DESs; the surface of a foamed nickel substrate is coated with a deep eutectic solvent DESs, heating treatment is carried out in an inert atmosphere, and the Cu3Ni / NF nanosheet self-supporting electrode is obtained. The preparation method is simple in preparation process, mild in condition, low in preparation cost, good in element compatibility, capable of achieving industrial production and free of pollution to the environment. And the obtained Cu3Ni / NF nanosheet self-supporting electrode has excellent electrocatalytic activity.

The present invention discloses a golden chrysanthemum flavonoid glycoside derived from golden chrysanthemum, wherein the golden chrysanthemum flavonoid glycoside is apigenin 7-O-(6"-O-malonyl)-β-D-glucoside derived from golden chrysanthemum. The present invention separates and purifies apigenin 7-O-(6"-O-malonyl)-β-D-glucoside from golden chrysanthemum for the first time, completes the first synthesis through a 5-step synthesis process with a total yield of 2.7%, and discovers for the first time that the compound has activity in improving hyperlipidemia and fatty liver in vitro and in vivo. Therefore, the compound can be used in the preparation of products for treating related diseases such as hyperlipidemia and fatty liver.

The present invention relates to a method of adding an isocitrate lyase specific inhibitor to a lactic acid fermentation process to block the production of succinic acid as a byproduct of fermentation. The specific inhibitor includes a combination of one or more of glycolic acid methyl ester, malonic acid dimethyl ester, hydroxymalonic acid diethyl ester, 3-nitropropionic acid ethyl ester, mercuric chloride, or 5,5'-dithiobis(2-nitrobenzoic acid) to effectively reduce the amount of succinic acid in the lactic acid.

Disclosed are a flux containing rosin, an active agent, and a solvent, the active agent containing an imidazole compound and two dicarboxylic acids, the two dicarboxylic acids being combined with malonic acid using one selected from succinic acid, adipic acid, and sebacic acid, and a method for preparing a joined body using the flux. Or the soldering flux contains rosin, an active agent and a solvent, the active agent contains an imidazole compound and two dicarboxylic acids, and the two dicarboxylic acids are combined with succinic acid and one selected from suberic acid, sebacic acid, methylsuccinic acid, malic acid and malonic acid. According to the present invention, it is possible to provide a flux capable of increasing the leg size and suppressing the occurrence of bridging during soldering.

The application belongs to the field of organic synthesis, and discloses a method for preparing chiral 2-(1,3-diarylallyl)malonate by using a Pd / phosphine oxygen bidentate phosphine phenol ligand catalysis, which comprises the following steps: under a protective atmosphere, mixing P, O-bidentate phosphine phenol ligand, a palladium catalyst, N, O-bis(trimethylsilyl)acetamide, a malonate nucleophilic reagent and an allyl acetate electrophilic reagent in dichloromethane, and reacting to obtain chiral 2-(1,3-diarylallyl)malonate product. The system has the advantages of high enantioselectivity, high catalytic efficiency, wide substrate application range and mild conditions.

The invention belongs to the technical field of medicine detection, and particularly relates to dipropyl malonic acid prepared by a dimethyl malonate method and a detection method of impurities of the dipropyl malonic acid. According to the detection method provided by the invention, the dipropyl malonic acid prepared by a dimethyl malonate method and impurities thereof are detected through high performance liquid chromatography (HPLC) for the first time; the impurities comprise propyl malonic acid, 2-methyl-2-propyl malonic acid, 2-propyl-2-butyl malonic acid, propyl malonic acid monomethyl ester, 2-methyl-2-propyl malonic acid monomethyl ester, dipropyl malonic acid monomethyl ester, 2-propyl-2-butyl malonic acid monomethyl ester, propyl malonic acid dimethyl ester, dipropyl malonic acid monopropyl ester and propyl malonic acid dimethyl ester; the invention relates to a method for preparing dipropyl malonic acid, which is selected from one or more of dipropyl malonic acid dimethyl ester, dipropyl malonic acid methyl ester propyl ester and 2-propyl-2-butyl malonic acid dimethyl ester, and solves the problems of quality control and process evaluation of dipropyl malonic acid serving as an intermediate of sodium valproate prepared by a dimethyl malonate method.

The invention discloses a method for catalytically synthesizing alpha-disubstituted ester, amide, malonic acid monoester or monoamide from disubstituted Meldrum's acid. By developing a new strategy for promoting the ring-opening reaction of the disubstituted Meldrum's acid by alkali, the disubstituted malonic acid monoester or monoamide can be efficiently prepared, and compared with the previous method, the strategy can obtain the target product at the room temperature at the yield of 99%. The method successfully breaks through the limitation of the existing disubstituted malonic acid monoester synthesis method, and enriches the types of target compounds. Besides, a series of novel disubstituted malonic acid monoesters are obtained, and simple chemical conversion is applied to obtain a series of disubstituted malonic acid derivatives with quaternary carbon centers. Then, under the action of a chiral organic catalyst, chiral disubstituted malonic acid monoester is obtained with high yield and high enantioselectivity. And a solid foundation is laid for subsequent application of the compounds in subjects of materials, medicines and the like.

The invention discloses a gram-level synthesis method of Dactyllactone A. The gram-level synthesis method of Dactyllactone A is shown in the description. The method comprises the following steps: with simple and easily available aryl iodide, aziridine and triisopropyl silylacetylene as starting materials, stirring and reacting in an organic solvent at 60-70 DEG C under the action of a palladium catalyst, a phosphine ligand, a norbornene derivative and alkali to obtain a key intermediate; the key intermediate is condensed with iodo gem-dimethyl ester furanone prepared from propiolic acid and dimethyl malonate iodine ylide, and then the condensation product is subjected to an Au / Ag catalyzed intramolecular hydroamination reaction, photocatalytic 6-pi electro-cyclization and two-step conversion, so that the natural product Dactyllactone A can be obtained, wherein the iodo gem-dimethyl ester furanone and iodo gem-dimethyl ester furanone are prepared from propiolic acid and dimethyl malonate iodine ylide. The method has the advantages of cheap and easily available raw materials, short reaction steps, high reaction efficiency, large preparation scale, simple preparation process and the like, has great application potential, and lays a good foundation for industrial production.

A teeth whitening composition comprises malonic acid or a salt thereof and a thickening system comprising xanthan gum, carrageenan, and about 1.5% or more thickening silica by weight of the composition. The teeth whitening composition has a film-to-clean ratio (PCR) value of at least 115.

The invention belongs to the field of organic chemistry, and particularly relates to a synthesis method of a rosuvastatin calcium key intermediate, which comprises the following steps: (1) taking (S)-4-chloro-3-hydroxybutyric acid as a raw material, and performing condensation ester with methanol under the condition of an esterification reaction condensing agent to obtain a compound with a structural formula B, and (2) taking the compound with the structural formula B as a raw material, and under the alkaline condition, performing condensation ester reaction to obtain the rosuvastatin calcium key intermediate. The preparation method comprises the following steps: (1) carrying out a reaction with tert-butyl malonate to obtain a compound with a structural formula C, (3) adding glucose and alkali into the compound with the structural formula C as a raw material under an enzyme catalysis condition to obtain a chiral reduction product D, and (4) heating the compound with the structural formula D as a raw material in the presence of only 2, 2-dimethoxypropane to obtain the rosuvastatin calcium key intermediate with a structural formula V. According to the method, tert-butyl bromoacetate and metal organic reagents which are high in cost and difficult to treat are not used, and solvents acetone and acid catalysts are not used in the ketal reaction, so that the production cost is reduced, and the method is more environment-friendly and efficient.

This invention discloses the preparation and gas adsorption separation application of pyrazole-3,4,5-tricarboxylic acid ligand heteronuclear metal-organic framework materials, comprising the following steps: 1) Weighing CuCl2·2H2O, Ba(NO3)2, and 1H-pyrazole-3,4,5-tricarboxylic acid as raw materials; 2) Placing the raw materials in a polytetrafluoroethylene-lined reactor, adding distilled water, and adjusting the pH to 2-4 with malonic acid; 3) Sealing the reactor and heating the reaction, raising the temperature from room temperature to 80-120℃ over 0-12 hours, holding the temperature for 70-75 hours, and then lowering it to room temperature over another 0-12 hours; 4) Collecting the product, washing, and vacuum drying to obtain the chemical formula [Cu2Ba(HL)2(H2O)3]. n The crystal is a pyrazole-3,4,5-tricarboxylic acid. By combining the multi-site coordination advantages, heterometallic node construction advantages, and pore functionalization control advantages of pyrazole-3,4,5-tricarboxylic acid, a stable framework structure can be constructed while simultaneously adjusting pore size, optimizing pore wall polarity, and constructing local adsorption sites, thereby enhancing the material's application potential in SF6 capture and separation, and C2 gas adsorption and storage.

The invention relates to the technical field of chemical cleaning agents, in particular to a cleaning agent for cleaning a SiC wafer and a preparation method of the cleaning agent. The cleaning agent for cleaning the SiC wafer is prepared from the following components in percentage by mass: 10 to 15 percent of an organic acid component, 6 to 12 percent of a surfactant, 4 to 6 percent of an auxiliary agent and the balance of water, the pickling component is prepared from monoethyl malonate, modified citric acid and aminosuccinic acid. Aiming at the problems that an existing cleaning agent is difficult to achieve efficient cleaning, the wafer surface is prone to being damaged, and the performance and the yield of a semiconductor device are affected, the cleaning agent with the better removal effect is prepared, the cleaning agent has high cleanliness and reliability, pollutant particles on the wafer surface are removed, and damage caused by secondary corrosion to the surface is prevented.

The present invention relates to a cellulose ester film comprising, in a cellulose ester substrate, a sesamolbenzotriazole-based first ultraviolet absorber and at least one second ultraviolet absorber selected from benzotriazole-based, malonate-based, triazine-based and benzophenone-based ultraviolet absorbers, and the cellulose ester film of the present invention uses both a long-wavelength first ultraviolet absorber containing an alkyl chain to ensure sufficient solubility and a second ultraviolet absorber for ensuring light resistance, and thus ensures both long-wavelength region absorption performance and light resistance reliability while having significantly low ultraviolet transmittance.

The invention discloses a method for preparing a fluorinated ethylene-propylene emulsion, and relates to a polymer emulsion polymerization technology. Comprising the following steps: adding water into a reaction kettle, heating, and replacing with nitrogen to control oxygen; adding perfluoropolyether ammonium carboxylate, heating, adding an initial TFE / HFP mixed monomer, stirring, and adding a potassium persulfate solution to initiate polymerization; supplementing the mixed monomer in the reaction to maintain the pressure, and adding diethyl malonate and a copolymerization composition regulator at the same time; and stopping the reaction after the designed feeding amount is reached. According to the invention, the proportion of copolymerization units can be optimized, high monomer conversion is realized, and the emulsion with high solid content and uniform particle size is obtained.

The application discloses a preparation method of ammonium glufosinate, which comprises the following steps: adding diethyl malonate and liquid bromine into a first solvent to react to obtain intermediate I; adding the intermediate I, potassium phthalimide and a quaternary ammonium salt catalyst into toluene to react to obtain intermediate II; adding the intermediate II, potassium carbonate, 1,2-dibromoethane and a phase transfer catalyst into a second solvent to react to obtain intermediate III; adding the intermediate III and diethyl methyl phosphonite into toluene to react under argon to obtain intermediate IV; adding the intermediate IV into hydrochloric acid to react under reflux; cooling, precipitation, drying to obtain intermediate V; mixing the intermediate V with water, passing in ammonia and adjusting pH value; adding methanol and stirring to react; cooling, filtering and drying to obtain ammonium glufosinate. The method can avoid using sodium cyanide or hydrocyanic acid, and no large amount of difficult-to-separate ammonium chloride is generated, the content of the obtained ammonium glufosinate is 90% to 98%, and the total yield is greater than 68%.

The invention relates to a blocked polyurethane composition based on at least one diisocyanate and / or polyisocyanate, at least one polyol, at least one hydroxyl chain extender and at least one end-capping agent, the at least one end-capping agent being selected from malonates, acetoacetates and acetylacetonates, and the at least one polyol is selected from the group consisting of polyester polyols, polycarbonate glycols, and polycaprolactone glycols; a use of the composition; the invention discloses a preparation method of an artificial leather surface layer and the artificial leather surface layer.

The application relates to a preparation method of 4-chloropyrrolopyrimidine, in particular to a four-step high-yield synthesis of 4-chloropyrrolopyrimidine by taking diethyl malonate and bromoacetaldehyde diethyl acetal as raw materials, through substitution reaction, then ring closure reaction with formamidine acetate, ring closure reaction under acidic conditions, and then chlorination reaction with phosphorus oxychloride; the preparation method of 4-chloropyrrolopyrimidine provided by the synthesis route is a preparation method with high yield, low cost, easy operation and suitability for industrialization.

New derivatives of 1-(4-methoxyphenyl)-7-oxo-6-[4-(2-oxopiperidin-1-yl) phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo [3,4c] pyridine-3-carboxamide (Apixaban) able to increase its water solubility. These derivatives are cocrystals derivatives ofApixaban of different acids, from which the most outstanding are the following: Apixaban Malonic Acid derivative, Apixaban-a-Ketoglutaric Acid derivative, Apixaban-Gallic Acid derivative, Apixaban-Maleic Acid derivative, Apixaban-L-Tartaric Acid derivative, and Apixaban Citric Acid derivative.