1010results about "Sulfide preparation" patented technology

The invention provides a novel method for synthesizing a fluoroalkyl substituted 4, 4 '-diaminodiphenylmethane compound, which comprises the following steps: under the action of a catalyst, reacting an amine compound with a fluorine-containing aldehyde compound in an organic solvent, and after the reaction is finished, carrying out post-treatment to obtain the fluoroalkyl substituted 4, 4'-diaminodiphenylmethane compound. The method has the advantages of mild reaction conditions, simple operation, high reaction efficiency, cheap and easily available raw materials, good atom economy, no generation of wastes, and large-scale application prospects. In addition, the fluoroalcohol solvent is recycled through simple distillation operation, the cost of a large amount of solvent is effectively saved, the process safety is improved, and efficient and green industrial production is facilitated.

The invention relates to a (methyl) acrylate monomer as well as a preparation method and application thereof, the structural general formula of the (methyl) acrylate monomer is as follows: # imgabs0 #, n is an integer of 1-20, and R1 is methyl or hydrogen; r2 and R3 are selected from hydrogen, Br, phenyl, methyl or # imgabs 1 #, wherein A1 in the # imgabs 2 # is phenyl or methyl. According to the (methyl) acrylate monomer provided by the invention, the molecular size of the whole monomer is relatively small, the whole monomer has a plurality of branched chain structures, the carbon chain length of a main chain is controllable, and the (methyl) acrylate monomer has high refractive index and good intermiscibility with other components.

Provided herein is a pleuromutilin derivative containing a cycloalkyl group and preparation method and application thereof. Specifically, the pleuromutilin is reacted with p-toluenesulfonyl chloride to obtain an intermediate I, and the intermediate I is reacted with 1-amino-2-methylpropane-2-thiol hydrochloride to obtain an intermediate II, and then the intermediate II is reacted with cycloalkylcarbonyl chloride to obtain a target derivative. The synthesis process of these derivatives is simple, with a high yield and simple purification. These derivatives can effectively inhibit activities of Staphylococcus aureus and Streptococcus, and have superior activities to the marketed Tiamulin, and they also have good antibacterial activities against drug-resistant bacteria. In particular, the treatment effect of the derivative 2 of the target derivative is significantly superior to the clinical drugs Tiamulin and Valnemulin. They are suitable as new antibacterial drugs for prevention and treatment of infectious diseases caused by bacteria in humans or animals.

The invention relates to an optical monomer and a preparation method and application thereof, the structural general formula of the optical monomer is as follows: R1, R2 and R3 are respectively selected from one of hydrogen and C1-C4 alkyl, A1 is selected from one of hydrogen and C1-C4 alkyl, and A2 is C1-C4 alkyl; r4 is selected from one of H, phenyl and C1-C4 alkyl, and A2 is C1-C4 alkyl; and R5 is hydrogen or methyl. The optical monomer provided by the invention contains a (methyl) acrylate group, and has the properties of high refractive index and low volume shrinkage; and a plurality of aromatic rings with high molar refractive index and low molar volume are contained, so that the whole molecule of the whole monomer is extremely high in refractive index. The monomer structure provided by the invention has a plurality of branched chains, the overall molecular weight is small, and the molecules are not easy to agglomerate.

The invention discloses a preparation method and composition of acetoacetic acid, 6-ethylthio-3-heptene-2-one and an intermediate thereof. Diketene is subjected to a hydrolysis reaction in water in the presence of a hydration catalyst to generate acetoacetic acid, wherein the hydration catalyst is soluble in water and is selected from a specific palladium, nickel, ruthenium or rhodium complex; acetoacetic acid and 3-ethylthiobutyraldehyde are subjected to a condensation reaction in the presence of a condensation catalyst to generate 6-ethylthio-4-hydroxy-2-one, and 6-ethylthio-4-hydroxy-3-carboxyl-2-one and 6-ethylthio-3-heptene-2-one may also be generated. The composition comprises the three products generated by the condensation reaction, and the product of the condensation reaction is reacted in a solvent in the presence of a dehydrating agent to prepare 6-ethylthio-3-heptene-2-one. The invention has simple operation, mild reaction conditions, no wastewater pollution to the environment, high atom utilization rate, high overall yield and good purity.

The invention discloses a (methyl) acrylate monomer, a holographic recording medium, a preparation method and a related device.The structural formula of the (methyl) acrylate monomer is as shown in G1-G5. The preparation method is easy to operate and high in synthesis yield, and further, the holographic recording medium can be applied to holographic recording. The (methyl) acrylate monomer with the structure is introduced into the photopolymer type holographic recording medium, reverse migration of a short polymer chain can be effectively inhibited, and therefore the holographic recording medium with high sensitivity and high diffraction efficiency is obtained, and the invention further provides a preparation method of the holographic recording medium. The invention also provides a volume holographic grating, a holographic optical element and an optical device comprising the holographic recording medium.

The invention relates to an optical monomer and a preparation method and application thereof, the structural general formula of the optical monomer is shown as G1, G2, G3 and G4, R1 and R2 are respectively selected from one of H, C1-C10 alkyl and halogen, A1 is C1-C10 alkyl, R3 is hydrogen or methyl, and n is a positive integer selected from 1-10. The optical monomer provided by the invention has a (methyl) acrylate group with high refractive index and low volume shrinkage property, contains a plurality of aromatic rings with high molar refractive index and low molar volume, and also has sulfur atoms with relatively high molar refractive index, so that the whole molecule of the whole monomer has extremely high refractive index. The whole monomer structure in the invention has at least two functionalities, and can realize fast reaction; the monomer structure also contains more branched chains and carbon chains, and molecules are not easy to agglomerate and have a certain migration rate.

The invention relates to a (methyl) acrylate monomer as well as a preparation method and application thereof, the structural general formula of the (methyl) acrylate monomer is shown as G1, G2 and G3: # imgabs0 #, r2 and R3 are selected from hydrogen, phenyl, methyl or # imgabs 1 #, wherein A1 in the # imgabs 2 # is phenyl or methyl. According to the (methyl) acrylate monomer provided by the invention, the molecular size of the whole monomer is relatively small, the whole monomer has a plurality of branched chain structures, the flexibility is good, the refractive index is high, and the intermiscibility with other components is good.

The invention discloses a 4, 4 '-bis (omega-alkenyl thioether) diphenyl sulfide monomer and a preparation method, the structural general formula of the 4, 4'-bis (omega-alkenyl thioether) diphenyl sulfide monomer is shown in the specification, n represents the number of methylene and is a positive integer, n = 1-10, the refractive index of a polymer obtained after the monomer and 4 '4-dimercapto diphenyl sulfide are polymerized is larger than 1.65 and smaller than 1.8, diffraction efficiency is remarkably improved, the preparation method is easy to operate, and the preparation method is suitable for industrial production. The invention further provides a photopolymer type holographic recording medium containing the monomer and a preparation method of the photopolymer type holographic recording medium, the sensitivity of the holographic recording medium is larger than 100 cm / mJ, the diffraction efficiency of a recording grating is larger than 95%, the refractive index modulation degree is larger than 0.1, the shrinkage rate is lower than 1%, and the preparation method is simple, controllable and suitable for industrial production. The invention also provides a volume holographic grating containing the holographic recording medium, a holographic optical element and an optical device.

The invention relates to an optical monomer and a preparation method and application thereof, the structural general formula of the optical monomer is shown as G1, G2, G3, G4, G5 and G6, R1 represents hydrogen, phenyl, halogen and C1-C4 alkyl, and A1 represents C1-C4 alkyl or phenyl; r2 represents hydrogen or methyl; n is a positive integer selected from 1-10. The optical monomer provided by the invention contains a plurality of aromatic rings with high molar refractive index and low molar volume, and also contains sulfur atoms with relatively high molar refractive index, so that the whole molecule of the whole monomer is extremely high in refractive index. The monomer structure provided by the invention has a plurality of branched chains, the overall molecular weight is small, and the molecules are not easy to agglomerate.

The invention discloses clethodim diamine salt as well as a preparation method and application thereof. The stability of the clethodim diamine salt (clethodim 1, 4-butanediamine salt, clethodim 1, 5-pentanediamine salt and clethodim 1, 6-hexamethylenediamine salt) provided by the invention is superior to that of clethodim and clethodim monoamine salt (such as clethodim tert-butylamine salt); meanwhile, the herbicidal activity of the clethodim diamine salt (clethodim ethylenediamine salt, clethodim 1, 4-butanediamine salt and clethodim 1, 5-pentanediamine salt) is superior to that of clethodim tert-butylamine salt, and the herbicidal activity of the clethodim 1, 5-pentanediamine salt is superior to that of clethodim. Most clethodim diamine salt is low in degradation rate in the high-temperature heat storage process and easier to store for a long time, the clethodim diamine salt is higher in melting point than clethodim monoamine salt (such as clethodim tert-butylamine salt), granulation and smashing are more convenient, the clethodim diamine salt can be used as a herbicide to be processed into solid dosage forms such as water dispersible granules and the like, the physical performance of the preparation is better, and the preparation has good application prospects. The commercialization prospect is good.

The present invention relates to process for preparing an aromatic amine (I) which comprises reacting an aromatic chloride (II) with an aminating agent (IV) selected from ammonia, an aliphatic or cycloaliphatic primary or secondary amine in the presence of a copper catalyst comprising copper and a ligand of the formula (III) or a salt thereof (III) where X, Y are identical or different and selected from the group consisting of halogen, OH, OR1, NH2, NHR2, N(R2)2, SH, SR3, SO3H, S(O)kR4 with k being 1, 2 or 3, where R1, R2, R3, R4 independently of each other are selected from the group of C1-C10 alkyl, C1-C10 haloalkyl, C3-C10 cycloalkyl, C6-C10 aryl and C6-C10 aryl-C1-C4-alkyl, where aryl in the last two mentioned moieties is unsubstituted or substituted by 1, 2, 3, 4 or 5 radicals Ra, where Ra is selected form F, CN, NO2, OH, SO3H, CH3, CF3 and OCH3; Z are both H or together form –CH=CH-.

This invention belongs to the field of veterinary drug technology, specifically relating to a 2,3-disubstituted naphthoquinone compound, its uses, and a preparation method. The 2,3-disubstituted naphthoquinone compound has the general formula: where X is selected from C, NH, O, and S; where X is selected from C, the X-R1 substituent represents an aryl substituent; when X is selected from NH, R1 is selected from hydrogen atom, C1-6 alkyl, C3-6 cycloalkyl, substituted aryl, substituted benzyl, or substituted acyl; when X is selected from O, R1 is selected from hydrogen atom, C1-6 alkyl, C3-6 cycloalkyl, C4-6 cycloalkyl, C5-6 cycloalkyl, C6-6 cyclo ... 3-6 cycloalkyl, substituted benzyl, substituted acyl; when X is selected from S, R1 is selected from C1-6 alkyl, substituted aryl, substituted benzyl; R2 is selected from C1-16 alkyl, substituted aryl, Ra-(CH2)n-, Ra-CO-(CH2)n-; This series of compounds has novel structures, excellent antiparasitic activity, and has been successfully applied in the field of veterinary drugs, solving long-standing safety and toxicity problems; its synthesis process is simple, the conditions are mild, and it can efficiently prepare a variety of 2,3-disubstituted naphthoquinone compounds.

The invention discloses an optical monomer and a preparation method thereof, a composition, a resin material and a preparation method thereof. The optical monomer provided by the invention comprises a quaternary carbon structure and a side chain connected with the quaternary carbon structure through an ester bond. The side chain comprises a thioether chain segment connected with an ester bond, an aromatic group connected with the thioether chain segment and an epoxy group connected with the thioether chain segment. The optical monomer provided by the embodiment of the invention takes a quaternary carbon structure as a core skeleton, and a side chain sequentially comprises an aromatic group, a thioether chain segment and a terminal epoxy group. A thioether structure with high polarizability and an aromatic group are introduced into the molecular design of the optical monomer, so that the refractive index and the optical transparency of a resin material are remarkably improved. And the rigidity of the epoxy aromatic ring is beneficial to improving the thermal stability and mechanical strength of the resin material. The epoxy group at the tail end can react with conventional epoxy resin to form a compact network structure, so that the stability of the resin material is improved, and the yellowing tendency is reduced.

A dimethyl sulfoxide synthesis system and a synthesis method, the system comprising: a fixed bed reactor (2) used to synthesize dimethyl sulfide, and an oxidation reactor (4) used to synthesize dimethyl sulfoxide. An external intensification unit (9) is disposed outside the oxidation reactor (4), the external intensification unit (9) comprising a first intensification reactor (901) and a second intensification reactor (902), the first intensification reactor (901) being disposed above the second intensification reactor (902), the first intensification reactor (901) being connected to a discharge port at a bottom end of the fixed bed reactor (2), the second intensification reactor (902) being connected to a nitrogen dioxide or oxygen storage tank (13), a connecting pipe (903) being disposed between the first intensification reactor (901) and the second intensification reactor (902), and a static mixer (904) being disposed in the connecting pipe (903).

The invention provides a bissanthin aromatic ring bay region C-H nucleophilic substitution reaction method and application thereof, and belongs to the field of organic synthesis methodology. According to the reaction, bissanthin is used as a raw material, dichloromethane and acetonitrile are used as solvents, and the bissanthin is oxidized by nitrite hexafluorotellurate and respectively reacts with nucleophilic reagents such as carbon anions, oxygen-containing reagents, sulfur-containing reagents, chlorine-containing reagents, nitrogen-containing reagents, phosphorus-containing reagents and cyano groups in one step to synthesize a series of bissanthin bay area modified functionalized products; when the reaction method is further applied to the nucleophilic substitution reaction of two molecules, namely perylene (Perylene) and N, N '-di (1, 3-diisopropyl benzene)-3, 4, 9, 10-perylene dicarboximide (PDI), good universality is shown, and the reaction method can be applied to the nucleophilic substitution reaction of two molecules, namely perylene (Perylene) and N, N'-di (1, 3-diisopropyl benzene)-3, 4, 9, 10-perylene dicarboximide (PDI). The method is mild in reaction condition, does not need to introduce transition metal as a catalyst, is easy in product separation and purification, and has the advantages of low cost, high efficiency and greenness; the series of functionalized derivatives constructed by the method can provide important intermediates for synthesis of larger polycyclic aromatic hydrocarbon molecules of the system; the method has a good industrial production prospect.

The invention discloses a preparation method of halogenated acrolein, which comprises the following steps: a compound shown as a formula V is prepared into a compound shown as a formula I under the combined action of a catalyst and an oxidizing agent, and the synthesis route is as follows: # imgabs0 #, and X is halogen. The method for preparing halogenated acrolein disclosed by the invention is mild in condition, high in yield and easy to industrialize. The invention further discloses application of the compound shown in the formula I in preparation of isoxazole, 2-hydroxypyrimidine and homopiperazine.

The invention discloses an acrylate monomer and a preparation method thereof, a photopolymer composition and a volume holographic grating and a preparation method thereof, the acrylate monomer provided by the invention is simple in structure and rich in expandable structure, so that the synthesis steps are simple and convenient, the cost is reduced, a relatively high refractive index of the monomer is realized on the basis of introduction of more sulfur atoms into the monomer, and the volume holographic grating has a good application prospect. In the subsequent photopolymerization process, the difference between the refractive index of the generated polymer and the refractive index of the common matrix is larger, so that the preparation of the holographic grating with high-refractive-index modulation degree can be realized.

The present invention discloses a tridentate pincer manganese complex, a preparation method thereof and an application thereof in alcohol dehydrogenation olefination reaction. The tridentate pincer manganese complex has the following structure: #imgabs0# wherein R is selected from a group containing C1-C 20 The method for preparing the tridentate manganese pincer complex comprises: using 8-aminoquinaldine as a raw material to synthesize a tridentate pincer ligand through multiple steps, and coordinating the tridentate pincer ligand with pentacarbonyl manganese bromide to prepare a novel tridentate manganese pincer complex. The tridentate manganese pincer complex prepared by the present invention has a novel skeleton structure, a simple and efficient preparation method, and high practicality. The obtained manganese complex has high activity as a catalyst in the dehydrogenation olefination reaction of alcohols and has very important application prospects.

The invention provides a photocuring composition and application thereof. The composition comprises the following components: (a) at least one benzoyl formate compound; (b) at least one ethylenically unsaturated photopolymerizable compound; the benzoyl formate compound is obtained by reacting a compound shown in a general formula (I) with a compound shown in a general formula (II) or a general formula (III), or is obtained by further reacting the compounds shown in the general formula (I), the general formula (II) and the general formula (III) with a compound with an end-capped substituent group for end capping. The sensitivity of the obtained product is not reduced compared with that of existing small molecules, and the hardness of the product is improved under LED curing.

The invention relates to the technical field of rubber, in particular to a bio-based plasticizer and a preparation method thereof, a rubber composition and a rubber product. The preparation method of the bio-based plasticizer provided by the invention comprises the following steps: reacting bio-based oil, a sulfur-containing compound, a photoinitiator and an organic solvent to obtain the bio-based plasticizer, the bio-based oil comprises grease containing unsaturated double bonds; the structural general formula of the sulfur-containing compound is R-SH; in the formula, R is selected from any one of substituted or unsubstituted alkyl and aralkyl of C1-C18. According to the preparation method of the bio-based plasticizer disclosed by the invention, the bio-based oil is modified by utilizing the sulfur-containing substance, and the content and activity of unsaturated double bonds in the bio-based oil are reduced, so that the influence of the unsaturated double bonds on a rubber vulcanization process is reduced, and the thermal stability and mechanical property of rubber are favorably improved; in addition, the prepared bio-based plasticizer has relatively low kinematic viscosity, and is beneficial to improving the operating performance of a rubber material.

This invention belongs to the field of chemical synthesis and relates to a method for achieving deuterated methylation of a nucleophile. The invention provides a deuterated methylating reagent, which is obtained by reacting formic acid with deuterated methanol under acidic conditions, followed by a second reaction with thiaanthracite and trifluoromethanesulfonic acid. The nucleophile is then reacted with the deuterated methylating reagent described in claim 1, a base, and a solvent to obtain the deuterated methylated product. This invention also provides a method for achieving deuterated methylation of a nucleophile, which involves dissolving the nucleophile and 5-deuterated methyl-5H-thiophene-5-onium trifluoromethanesulfonate in a suitable solvent, adding a base, and then performing the deuterated methylation reaction at room temperature. In the method provided by this invention, the yield of the product after nucleophile methylation can reach 52% to 95%.

The invention discloses a synthesis method of an N-formamide derivative, and belongs to the technical field of chemical synthesis, the N-formamide derivative is obtained by a one-step method by taking an isonitrile compound as a substrate and a titanocene compound as a catalyst and carrying out hydrolysis reaction in an organic solvent at room temperature and normal pressure. According to the method, the titanocene compound is used as a catalyst, and the hydrolysis reaction is selectively terminated to the step of generating the formamide compound in the isonitrile compound hydrolysis process, so that the isonitrile compound is prevented from being further hydrolyzed to generate the amine compound. The method has the advantages of simple reaction process, cheap and easily available reaction system, wide substrate range, mild reaction conditions, high target product yield and no burden on the environment.

The invention provides a high-temperature-resistant bactericidal corrosion inhibitor as well as a preparation method and application thereof. The preparation method comprises the following steps: reacting a sulfydryl carboxylic acid compound and polyethyleneimine in an organic solvent at a first temperature for a first time to obtain a system containing a first compound; and adding halogenated hydrocarbon into the system containing the first compound, reacting at a second temperature for a second time to obtain a system containing a second compound, removing the organic solvent, and drying to obtain the high-temperature-resistant bactericidal corrosion inhibitor. The high-temperature-resistant bactericidal corrosion inhibitor disclosed by the invention is prepared by the preparation method. The invention also provides an application of the high-temperature-resistant bactericidal corrosion inhibitor in microbial corrosion protection and / or chemical corrosion protection of oil and gas fields. The high-temperature-resistant bactericidal corrosion inhibitor disclosed by the invention is simple in preparation method, good in high-temperature stability and excellent in bactericidal corrosion inhibition performance.

The invention relates to the technical field of organic sulfide preparation, in particular to a method for synthesizing and refining dimethyl sulfide (DMS) and dimethyl sulfoxide (DMSO) embedded into a methanol plant, which mainly utilizes high-purity oxygen of an air separation unit of the methanol plant, a high-concentration hydrogen sulfide product of low-temperature methanol washing and part of top gas-phase refined methanol of a pressurizing tower of a methanol rectification device. The production cost of the product is reduced, the added value of the product is improved, and the hydrogen sulfide product of a methanol plant is effectively utilized.

The present invention relates to a method for large-scale production of a benzo [d] thiazole intermediate for preparing torametinib, and a method for large-scale preparation of torametinib using the intermediate, the method avoiding a column chromatography operation which is expensive and complicated to operate while significantly improving the yield of the benzo [d] thiazole intermediate, and the method for large-scale production of torametinib using the intermediate. And thus, the yield of the final product torametinib is improved. Therefore, according to the method, the cost is greatly reduced, the yield is improved, and the method is suitable for large-scale production.

The invention discloses a preparation method of tiamulin and tiamulin fumarate based on Bunte salt, which comprises the following steps: mixing the Bunte salt and pleuromutilin p-toluenesulfonate, reacting at 45-65 DEG C for 3-5 hours to synthesize tiamulin, preparing the Bunte salt through a reaction formula 1, and preparing the pleuromutilin p-toluenesulfonate through a reaction formula 2, the molar ratio of the 2-diethylaminoethanol to the sodium thiosulfate to the chlorination reagent in the reaction formula 1 is 1: (1-1.3): (1-1.5), and the molar ratio of the pleuromutilin to the paratoluensulfonyl chloride to the pyridine in the reaction formula 2 is 1: (1-1.2): (1-1.2); the prepared tiamulin and fumaric acid are used as raw materials for a salt forming reaction, the reaction temperature ranges from 55 DEG C to 65 DEG C, the reaction time ranges from 40 min to 80 min, and after the reaction is finished, the tiamulin fumarate is prepared through cooling, crystallization, centrifugation and drying; the tiamulin fumarate disclosed by the invention is high in content, low in total amount of impurities, few in variety and stable in quality under high-temperature and high-humidity conditions, and the preparation method is simple and easy to operate and good in product quality.

The present invention provides a novel method for producing a derivative of an organic substance that contains one or more groups selected from the group consisting of a sulfanyl group, a selanyl group and a sulfino group. A method for producing a derivative of an organic substance, said method comprising a process for obtaining a derivative of an organic substance that contains one or more groups selected from the group consisting of a sulfanyl group, a selanyl group and a sulfino group by reacting the organic substance with an olefin compound under acidic conditions. With respect to this method for producing a derivative of an organic substance, the olefin compound contains an ethylene structure that has at least two electron-withdrawing groups (excluding halogen atoms).

The invention belongs to the technical field of organic synthesis, and discloses a synthesis method of a disulfide compound. According to the invention, under the catalytic action of 1, 4, 7, 10, 13, 16-hexaoxacyclo-octadecane, halogenated hydrocarbon, sodium sulfide and sulfur react at the temperature of 50-60 DEG C to prepare the disulfide compound. The synthesis method of the disulfide compound has the advantages of being simple in process, small in catalyst dosage, mild in reaction condition, high in production efficiency, low in production cost, convenient for industrial production and the like, in addition, the reaction yield of the synthesis method can reach 94.8%-96.6%, and the purity of the obtained target product reaches up to 97.9%-99.3%. The method can be applied to preparation of the disulfide compound, and the obtained disulfide compound can be further applied to the fields of biomedicine, agriculture, chemical industry and the like.

The present application provides a method for preparing copper methionine from a methionine intermediate and copper methionine, and relates to the technical field of feed additive preparation. The method for preparing copper methionine from a methionine intermediate comprises: obtaining a sodium methionine solution and a copper sulfate solution; adjusting the pH of the sodium methionine solution; adding the copper sulfate solution to the sodium methionine solution for a chelation reaction to obtain a copper methionine solution; separating the copper methionine solution to obtain a copper methionine filter cake and a filtrate; and drying the copper methionine filter cake to obtain a copper methionine product. The synthesis of copper methionine with sodium methionine solves the problem of the complex synthesis process of sodium methionine chelating copper methionine, allowing the mother liquor to be recycled, saving costs while reducing harm to the environment.