753results about "Sulfide preparation" patented technology

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 (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 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.

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.

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.

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 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 invention discloses a preparation method of dimethyl thio toluenediamine, which comprises the following steps: continuously introducing dimethyl disulfide into a reaction system containing diaminotoluene and a catalyst for reaction, and evaporating and condensing the dimethyl disulfide in the reaction process so as to bring out a byproduct methyl mercaptan, after the reaction is finished, purifying and decoloring by adopting a neutralization distillation method to obtain dimethyl thio toluenediamine; the neutralization distillation method comprises the following steps: adding dimethyl disulfide into a reaction solution after the reaction is finished for dilution, then filtering the reaction solution to obtain a filtrate, adding an alkali solution into the filtrate for neutralization, heating and stirring, and finally carrying out reduced pressure distillation. The preparation method disclosed by the invention has the advantages of small catalyst dosage, short reaction time, high product yield and economic and environment-friendly purification and decoloration modes.

The invention belongs to the technical field of synthesis and preparation of high-molecular optical materials, and particularly relates to a multi-mercaptothiol composition as well as a preparation method and application thereof. According to the present invention, the three-step synthesis route of the tetrahydroxymethylation reaction, the thiol precursor introduction and the deprotection is adopted, the reaction conditions are mild, the steps are clear, the yield is high, the complexity of the traditional synthesis route is avoided, the production cost is reduced, and the industrial production is easily achieved. In the aspect of refractive index regulation and control, the compound contains a plurality of sulfur atoms, the coating is endowed with the characteristic of high refractive index, accurate regulation of the refractive index can be realized by adjusting the formula of the composition, the requirements of different optical applications are met, and the application range of the material is widened. The prepared optical coating has excellent light transmittance, light loss can be reduced to the maximum extent, and the efficient performance of an optical device is ensured; meanwhile, the haze value of the coating is low, the light scattering phenomenon is effectively avoided, and the imaging definition and the precision of an optical system are guaranteed.

The invention discloses an optical monomer, a holographic recording medium, a preparation method and a related device, the structural general formula of the optical monomer is as shown in G1-G6, the monomer is high in refractive index, the preparation method is simple, and further, the optical monomer with the structure is introduced into the photopolymer type holographic recording medium, so that the photopolymer type holographic recording medium is prepared. The invention further provides a preparation method of the holographic recording medium, a volume holographic grating containing the holographic recording medium, a holographic optical element containing the holographic recording medium and an optical device containing the holographic recording medium.

The invention belongs to the technical field of organic light-emitting materials, and particularly relates to a step-by-step stimuli-responsive crystalline light-emitting material and a preparation method and application thereof. The crystalline luminescent material is a crystalline material based on a polysulfide aromatic hydrocarbon type compound, and the polysulfide aromatic hydrocarbon type compound is a compound based on a tetrathiobenzene mother nucleus. The compound does not have a photoluminescence discoloration property in a crystalline state, but has an obvious photoluminescence discoloration property after the crystallinity is reduced through force stimulation; and the wavelength and proportion of fluorescence / phosphorescence of the compound and the molecular orbital of an excited state can be controlled by adjusting related substituents, so that the optical property is adjustable. The high-crystallinity material prepared from the compound has a response effect on step-by-step stimulation of force and light, so that the high-crystallinity material can be applied to encryption anti-counterfeiting, information storage and the like. The application scenarios include currency anti-counterfeiting, certificate anti-counterfeiting, commodity package anti-counterfeiting, bill anti-counterfeiting, artwork anti-counterfeiting, electronic equipment anti-counterfeiting, logistics anti-counterfeiting, supply chain anti-counterfeiting and the like.

The invention discloses a modified polymer cement-based normal-temperature foaming fireproof coating and a preparation method thereof, and relates to the technical field of fireproof coatings. The modified polymer cement-based normal-temperature foaming fireproof coating comprises a component A and a component B, the component A is prepared from the following raw materials in parts by weight: 15 to 20 parts of cement, 10 to 12 parts of calcium carbonate, 0.3 to 0.9 part of nano titanium dioxide, 30 to 35 parts of polyurethane emulsion, 1 to 2 parts of cross-linking agent, 8 to 12 parts of flame retardant, 1 to 3 parts of foaming agent, 0.5 to 1.5 parts of dispersing agent and 10 to 20 parts of deionized water; the component B comprises the following raw materials in parts by weight: 20-25 parts of a curing agent, 0.1-0.5 part of an organic zinc catalyst and 0.5-1.2 parts of a foam stabilizer; the prepared modified polymer cement-based normal-temperature foaming fireproof coating has excellent fireproof performance, bonding strength and compressive strength.

The application discloses a preparation method of perfluoroalkyl aryl sulfide, and a structural formula of the perfluoroalkyl aryl sulfide is shown as formula (I); the method comprises the following steps: firstly, obtaining corresponding aryl sulphenyl chloride by chlorination of thiophenol; under the condition that fluoride and crown ether exist, obtaining perfluoro-1,1-dimethylbutyl negative ion by addition of D-2 ‑ And the aryl sulphenyl chloride added is subjected to a nucleophilic substitution reaction to synthesize a product (1,1,1,3,3,4,4,5,5,5-decafluoro-2-trifluoromethylpent-2-yl)(aryl)sulfide. The application adopts a reaction strategy of efficient coupling of thiophenol and perfluoroalkyl, and can be used for preparing various fluorine-containing benzene sulfide compounds.

The invention provides a synthesis method of a thioether ligand and a palladium-catalyzed 2-aryl indole compound, and designs an application of the biphenyl thioether ligand and a palladium catalyst in preparation of the 2-aryl indole compound. Indole and arylboronic acid are subjected to a reaction under the action of a palladium catalyst and a biphenyl sulfide ligand, and the structural formula of the biphenyl sulfide ligand is shown in the specification. Ar is phenyl, furyl, thienyl, naphthyl or phenyl substituted by one or more substituent groups; r1 is methyl, methoxyl, fluorine atom, chlorine atom, bromine atom or methyl ester group; r2 is the same or different and is methyl, ethyl, isopropyl, isobutyl, cyclohexyl, benzyl, n-butyl or n-hexyl; r3 is alkoxy, alkylthio, substituted amino or halogen; the palladium catalyst is a divalent palladium compound.

The present application relates to a kind of preparation method of vicinal diol compound, which comprises the following steps: in non-aqueous solvent, formula (I) compound and reducing agent are reacted under light condition, to obtain the vicinal diol compound shown in formula (II);The reducing agent is formic acid or formate;The wavelength of the light is less than 390nm;Its reaction formula is as follows.The preparation method of the present application does not need transition metal catalyst, also does not need other special catalyst and special additive, and the aldehyde ketone substrate can be reacted with formic acid or formate in solvent by specific wavelength of light, to obtain corresponding vicinal diol compound with high yield, its reaction condition is mild, has wide substrate applicability, and green and environmental protection, simple and practical operation method, provides an effective synthesis strategy for the synthesis of shikimic alcohol compound.

The invention discloses a polyfunctional rosin-based reactive diluent. The structural formula of the polyfunctional rosin-based reactive diluent is shown as a formula (I) or a formula (II). The polyfunctional rosin-based reactive diluent has a rigid tricyclic diterpenoid structure of rosin, is small in molecular weight and low in viscosity, can be used for preparing an ultraviolet curing material, has excellent hardness and scratch resistance after light curing and film forming, and is simple in preparation method, low in cost and suitable for industrial production. And a polycarboxylic acid functional group is efficiently constructed under a mild condition.

The invention belongs to the field of agricultural acaricides. In particular to a phenyl sulfide (sulfoxide) compound and application thereof. The structure is shown as a general formula I, wherein the definition of each substituent group in the formula # imgabs0 is shown in the specification. The compound as shown in the general formula I has excellent acaricidal activity and can be used for preventing and treating various pest mites.

The invention discloses a photocatalytic synthesis method of diethyl disulfide, and relates to the technical field of organic synthesis. The preparation method specifically comprises the following steps: mixing Co (NO3) 2.6 H2O and Ni (NO3) 2.6 H2O, and adding methanol to obtain a solution A; 2-methylimidazole and methyl alcohol are mixed, and a solution B is obtained; mixing the solution A and the solution B to obtain a zeolite imidazole framework material; selenium powder and the zeolite imidazole framework material are mixed and calcined, and a NiCoSe2 material is obtained; the preparation method comprises the following steps: mixing a NiCoSe2 material, ZnCl2, InCl3 and C2H5NS, adding an ethanol water solution, and carrying out microwave hydrothermal synthesis to obtain a NiCoSe2-coated ZnIn2S4 photocatalyst; the NiCoSe2-coated ZnIn2S4 photocatalyst and ethanethiol are subjected to a photocatalytic reaction under N2 atmosphere protection and visible light irradiation, and diethyl disulfide and hydrogen are generated. The method is mild in reaction condition and high in product stability.

The present application provides a method for preparing a deuterated chemical by means of a deuteration reaction of a carbon-hydrogen bond with a deuterium gas under the catalysis of an alkali, wherein in the presence of a catalyst, a deuterium gas is added into a compound containing a carbon-hydrogen bond for a deuteration reaction so as to generate a deuterated compound. A deuterium gas is used as a deuterium source, such that multiple water separation operations, tedious steps and the wasting of energy caused by usage of a large amount of deuterium oxide as a deuterium source are avoided. Moreover, a cheap and easily available alkali metal compound is used for replacing an expensive transition metal catalyst and a complex-structure ligand as a catalyst for a deuteration reaction, and the alkali metal compound has the advantages of a low cost, a good compatibility with functional groups of a substrate and a high deuteration rate. The present application provides a new, low-cost, green and efficient deuteration method, which has a high application value.

The application provides a Pd6(SR) 12 cluster with an octahedral structure, the Pd6(SR) 12 cluster is a cyclohexanethiol ligand-protected palladium cluster, contains 6 Pd atoms, 12 cyclohexanethiol ligands, the 6 Pd atoms form an octahedral core, and the sulfur atoms in the cyclohexanethiol ligands are connected with the Pd atoms peripherally, and each sulfur atom is connected with two Pd atoms. The application further discloses a preparation method of the Pd6(SR) 12 cluster, and the application fills the technical vacancy of synthesizing Pd clusters with structures other than a ring structure, and has high popularization value.

The application discloses a preparation method of a key intermediate of dapagliflozin, and belongs to the technical field of preparation of medical intermediates. The preparation method of the key intermediate of dapagliflozin comprises the following steps: 1, 1-ethoxy-4-methylbenzene is prepared by using p-cresol, sodium hydroxide and diethyl sulfate; 2, (4-ethoxybenzyl) phenyl sulfide is prepared by using 1-ethoxy-4-methylbenzene, thiophenol, a palladium catalyst, an alkali and an oxidant; 3, 1-benzyl-4-ethoxybenzene is prepared by using (4-ethoxybenzyl) phenyl sulfide under a hydrogen atmosphere; 4, 4-ethoxy-2'-chlorobenzhydrol is prepared by carrying out chlorination reaction on 1-benzyl-4-ethoxybenzene; and 5, 5-bromo-2-chloro-4'-ethoxybenzhydrol is prepared by carrying out bromination reaction on 4-ethoxy-2'-chlorobenzhydrol. The yield and purity of 5-bromo-2-chloro-4'-ethoxybenzhydrol prepared by the method are higher, the process is safer, and the production cost is reduced.

The application discloses a full synthesis method of clethodim, and the method is characterized by reasonable selection / design of a process route, simplified process flow, reduced separation and purification operation, effectively reduced production cost and improved production efficiency, further improved yield of a key intermediate through research and screening of process conditions of the key step, reduced generation of impurities, and improved product quality and yield of the target product.