430 results about "Substitution reaction" patented technology

The invention provides a preparation method of a bexagliflozin intermediate, and relates to the technical field of organic synthesis. The preparation method provided by the invention comprises the following steps: S1, substitution reaction: under the action of alkali, carrying out substitution reaction on 2-(cyclopropoxy) ethanol and a compound III ((5-halogen-2-chlorphenyl) (4-halophenyl) ketone) to generate a compound II; s2, reduction reaction: under the action of lewis acid, carrying out reduction reaction on a reducing agent and a compound II ((5-halogen-2-chlorphenyl) (4-(2-(cyclopropoxy) ethyoxyl) phenyl) ketone) to generate a compound I; the method has the advantages of mild reaction conditions, high atom utilization rate, high yield, high product quality and the like.

The invention provides a preparation method and application of an asymmetric dicyclopentadienyl dialkoxy zirconium compound, and the preparation method comprises the following steps: (1) mixing a solvent with ZrCl4 and sodium cyclopentadienyl CpNa, and carrying out a reaction to obtain CpZrCl3; (2) the CpZrCl3 obtained in the step (1) and R1 substituted sodium cyclopentadienyl R1CpNa are subjected to a mixed reaction, and (R1Cp) CpZrCl2 is obtained; and (3) mixing the (R1Cp) CpZrCl2 obtained in the step (2) with alkoxy sodium salt R2Na, and carrying out a reaction so as to obtain the asymmetric dicyclopentadiene dialkoxy zirconium compound. According to the method, the substitution reaction of three sodium salts is used for replacing the ligand replacement reaction in the prior art, so that the reaction steps are shortened, the use of unnecessary raw materials is avoided, the production cost is reduced, and the obtained target product is high in yield and high in purity.

The invention relates to the technical field of organic dyes, in particular to a novel xanthene dye for blue photoresist color paste and a synthesis method of the novel xanthene dye. The invention relates to a synthesis method of a novel xanthene dye for blue photoresist color paste, which comprises the following steps: 1) taking rigid cyclic amine as a nucleophilic reagent, and carrying out aromatic nucleophilic substitution reaction on a chlorinated xanthene compound to obtain a xanthene intermediate; 2) performing chlorination reaction on the xanthene intermediate by using a chlorination reagent to obtain a chlorinated xanthene intermediate; 3) mixing active amine and the chlorinated xanthene intermediate, and performing substitution reaction under the action of alkali to obtain the novel xanthene dye for the blue photoresist color paste.The novel xanthene dye for the blue photoresist color paste.The novel xanthene dye for the blue photoresist color paste.The novel xanthene dye for the blue photoresist color paste.The novel xanthene dye for the blue photoresist color paste has the advantages of being high in solubility, good in thermal stability and high in contrast ratio.

The invention discloses a sulfide solid electrolyte of a lithium ion battery, comprising: a sulfide solid electrolyte matrix comprising sulfur; the surface of the sulfide solid electrolyte matrix is coated with the coating layer, and the coating layer is formed by substitution reaction of metal chloride, 1-undecyl mercaptan and sulfur. The sulfide solid electrolyte disclosed by the invention is a sulfide solid electrolyte with high ionic conductivity and good interface stability at the same time. The invention also discloses a preparation method of the sulfide solid electrolyte, a composite sulfide solid electrolyte and a preparation method of the composite sulfide solid electrolyte.

The invention provides a method for catalyzing hydrogen-deuterium replacement of heterocyclic aromatic hydrocarbon by using a binary cheap metal, and belongs to the technical field of organic synthesis.The method comprises the steps that a heterocyclic aromatic hydrocarbon compound serves as a raw material, heavy water and a binary cheap metal catalyst are added under the condition that a solvent is added or not added, under inert gas protection, heating is conducted for hydrogen-deuterium replacement reaction, and after the reaction is finished, a product is obtained; and separating and purifying the product to obtain the heterocyclic aromatic hydrocarbon deuterated compound. The preparation method provided by the invention adopts cheap heavy water as a deuterium source and cheap double-element metal as a catalyst, so that the cost is low, the operability is high, the applicability is wide, and the deuteration rate is high; a cheap and efficient heterocyclic aromatic hydrocarbon deuteration technology is realized, and the limitation of the existing heterocyclic aromatic hydrocarbon deuteration technology is solved.

The invention discloses a phototherapy reagent and a preparation method and application thereof. The preparation method comprises the following steps: 1-[4-(diethylamino) phenyl]-ethane-1-ketone and 4-methoxybenzaldehyde are subjected to a condensation reaction in a NaOH ethanol solution, and a product and nitromethane are subjected to addition; performing condensation and addition on the other groups of raw materials by the same method; cyclizing the two addition products with ammonium acetate, and coordinating with boron trifluoride diethyl etherate to obtain NHM; carrying out substitution reaction on the NHM and sodium nitrite to obtain NOO; and oxidizing NOO by m-chloroperoxybenzoic acid to obtain NNOO. The reagent can target a tumor hypoxia microenvironment, hypoxia monitoring is achieved, NO is released through photostimulation for tumor gas therapy, meanwhile, the secondary amplification photo-thermal therapy effect is achieved, preparation is controllable, diagnosis and treatment are integrated, and the reagent is sensitive, safe and suitable for biomedical research and clinical diagnosis.

The invention discloses an ultrasonic response quaternary ammonium salt polymer antibacterial agent and a preparation method thereof. The ultrasonic response quaternary ammonium salt polymer is prepared by the following steps: carrying out substitution reaction on azodiisobutylimidazoline and acryloyl chloride, then carrying out addition polymerization reaction with 4-aminomethylpiperidine, and then carrying out quaternization reaction with bromohexane. The obtained ultrasonic response quaternary ammonium salt polymer can be decomposed under the ultrasonic action to generate alkyl radicals, and has the sterilization effect. In addition, quaternary ammonium salt modification can improve the water solubility and the positive charge density of the polymer, and further improves the antibacterial performance.

The present invention relates to a preparation method for a novel benzylsulfinylpyridine compound, comprising using fluoropyridine, which contains electron-withdrawing substituents (such as halogen, trifluoromethyl, nitro, and cyano groups), as a starting material, and carrying out a substitution reaction and an oxidation reaction to obtain benzylsulfinylpyridine. According to the preparation method, a series of novel benzylsulfinylpyridine compounds can be obtained.

The application discloses a multifunctional biological imbibition agent and a preparation method and application thereof. The preparation method of the multifunctional biological imbibition agent comprises the following steps: (S1), alkylization reaction to obtain alkyl naphthalene; (S2), chloromethylation reaction to obtain halomethyl alkyl naphthalene; (S3), halogen alkyl nucleophilic substitution reaction to obtain hydroxymethyl alkyl naphthalene; and (S4), esterification reaction to obtain the multifunctional biological imbibition agent. The application further discloses application of the multifunctional biological imbibition agent as an imbibition agent in shale oil reservoir oil extraction. The application has the following advantages: (1) the reservoir adsorption amount is small, but the good wetting reversal characteristic is still maintained, and the emulsification is weak; (2) the high-temperature resistance is strong, and the temperature resistance reaches above 200 DEG C; (3) the preparation process is simple, and the yield is high; (4) the dosage is small, the cost is low, and the economic benefit is remarkable.

The application provides a synthesis process of metrafenone, in which inorganic alkali KOH is used as a catalyst, a key intermediate 4-(((5,5-dimethyl-dihydroisoxazole-4-yl)thio)methyl)-1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-ol can be obtained at low production cost and high yield, metrafenone is prepared through substitution reaction and oxidation reaction, the reaction yield is high, raw materials are simple and easy to obtain, three-waste emissions are small, and the process is beneficial to industrial mass production.

This invention belongs to the field of catalyst technology, providing a CO purification oxygen-rich catalyst, its preparation method, and its application. The preparation method involves dispersing γ-alumina in water, then sequentially adding copper nitrate and cerium nitrate to obtain a reaction solution. The reaction solution is mixed with an inorganic base, followed by a substitution reaction and a crystallization reaction to obtain a catalyst precursor. The catalyst precursor is calcined under a reducing atmosphere to obtain the CO purification oxygen-rich catalyst; the reducing atmosphere includes hydrogen. This preparation method generates sufficient active sites through a copper-cerium binary system, and then utilizes the basic groups provided by the inorganic base to form a low-valence metal-hydroxyl composite structure under a reducing atmosphere. Through the combined action of metal atoms, hydroxyl groups, and active oxygen sites, the research goals of high efficiency, stability, high selectivity, and economy are achieved. Furthermore, this preparation method does not use precious metals, resulting in low cost.

This invention provides a method for preparing and applying a highly insecticidal diamide compound, relating to the chemical and pesticide fields. The method includes: reacting 2-fluoro-3-nitrobenzoic acid with thionyl chloride (a chlorinating agent) and dimethylformamide (a catalyst) to obtain compound A; condensing compound A with 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline amide to obtain compound B; reducing compound B to obtain compound C; and, during the reaction under a hydrogen atmosphere, determining the reaction temperature and hydrogen flow rate in each hydrogenation reaction zone based on the concentration of compound B; reacting compound C with paraformaldehyde to obtain compound D; chlorinating 3-chloro-4-fluorobenzoic acid with thionyl chloride (a chlorinating agent) and dimethylformamide (a catalyst) to obtain compound E; and amide condensing compound E with compound D to obtain the novel diamide compound of this invention. The diamide compound of this invention exhibits excellent insecticidal effects when used in pesticide compositions.

The invention provides a preparation method of a dihalo-substituted dibenzo [b, f] aza-5-formyl chloride compound, which is prepared from a compound II through dihalo substitution reaction. The method is reasonable in process, high in reaction yield and suitable for large-scale industrial production. In the reaction formula, R1 can be a halogen substituent such as bromine, chlorine or iodine, and R2 can be H, C1-C6 alkoxy and the like.

The invention discloses an acrylic acid silane ester self-renewal antifouling resin based on cation-pi interaction as well as a preparation method and application of the acrylic acid silane ester self-renewal antifouling resin. Methyl methacrylate, ethyl acrylate, triisopropylsilyl methacrylate, acrylic acid-2-methyl ethyl ester, paeonol methacrylate and acryloyloxyethyl trimethyl ammonium chloride are synthesized through a random free radical polymerization reaction with azodiisobutyronitrile and benzoyl peroxide as initiators. Wherein the methacrylic acid paeonol ester monomer is prepared by carrying out substitution reaction on paeonol and methacryloyl chloride. The anti-fouling agent is anchored on the surface of the coating again through cation-pi interaction, so that the anti-fouling effect is enhanced, and the coating still has good anti-fouling capacity even in a static environment.

The application relates to the technical field of organic synthesis, and discloses a synthesis method of benzthiazuron, which comprises the following steps: step 1, addition reaction of alpha-methyl styrene and hydrogen chloride gas, and degassing to obtain a first reaction liquid; step 2, substitution reaction of the first reaction liquid and cyanate in the presence of a zinc chloride catalyst, and filtration to obtain a second reaction liquid containing isocyanate; and step 3, construction of an inorganic salt aqueous solution system with a density of 1.05-1.10 g / ml and a pH of 9-10, dropwise addition of the second reaction liquid into the system for condensation reaction with o-chlorobenzylamine, and post-treatment and refinement to obtain a target product. The non-phosgene route of chloro-isocyanate substitution is adopted, and the use of the toxic phosgene is completely avoided; the salting-out effect and interface control generated by the specific high-density salt solution effectively inhibit the isocyanate hydrolysis side reaction, and the reaction yield and product purity are obviously improved.

The invention relates to the technical field of chemical synthesis, and particularly discloses an indolone compound and a preparation method thereof. The structure of the indolone compound is shown as a formula (I). The one-step substitution reaction-based indolone compound preparation method provided by the invention has the outstanding advantages of mild reaction conditions, simple operation steps, high product yield and the like, and effectively overcomes the common problems of tedious steps, harsh conditions, poor selectivity and the like in the existing synthesis route. Establishment of an efficient synthesis route provides a reliable way for rapid and large-scale preparation of indolone derivatives with novel structures. The series of novel indolone compounds with potential excellent biological activity provide a new opportunity for discovery of innovative drug lead compounds and development of novel functional materials, and have important research value and wide application prospects. Formula (I)

This invention discloses a magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd, its preparation method, and its applications. Using an amino alcohol as a starting material, an imidazole derivative containing a hydroxyl group on the N-substituent is obtained through a condensation and ring-closing reaction. This derivative is then subjected to substitution reactions with thionyl chloride and cyclohexanethiol sequentially to obtain an imidazole derivative containing a thioether on the N-substituent. This derivative is then reacted with 1,3-dibromopropane to obtain an N-bromopropyl-N'-cyclohexane thioether-substituted imidazole bromium salt. This salt is then reacted with Pd(OAc)₂ or PdCl₂ via a direct metallization reaction to obtain the N-bromopropyl-substituted thioether-chelated nitrogen heterocyclic carbene palladium complex NHC-Pd. The NHC-Pd complex is then reacted with amino-functionalized magnetic nanoparticles (MNPs-NH₂) to prepare the magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd. It not only possesses the activity of homogeneous nitrogen heterocyclic carbene palladium catalysts, but also has a simple synthesis method, high yield, and is easy to separate and reuse in catalytic C-C bonding reactions, showing good application prospects in the field of catalysis.

The invention belongs to the field of pharmaceutical chemicals, and relates to a preparation method of an anti-influenza virus derivative intermediate. According to the invention, a compound (a) and a compound (b) are taken as initial raw materials, and an alcoholic hydroxyl group is directly converted into an active intermediate by utilizing trimethylsilyl trifluoromethanesulfonate (TMSOTf), so that the tedious operation of firstly protecting the hydroxyl group and then carrying out substitution reaction in the traditional method is avoided, and a key intermediate (d) required for preparing the anti-influenza virus derivative can be obtained in one step. The method has the advantages of simplicity and convenience in operation, high yield, easiness in industrial amplification and the like, and is suitable for large-scale preparation of the anti-influenza virus medicine and pharmaceutically acceptable salts, esters or solvates thereof.

The application belongs to the technical field of medicine, and relates to N-methyl-2-(9-oxoacridin-10(9H)-yl)acetamide compounds and a preparation method and application thereof. The preparation method of the compound is as follows: taking o-aminobenzoic acid as a starting material, performing substitution reaction, condensation reaction, alkylation reaction and hydrolysis reaction to generate a key intermediate acridone acetic acid, and finally performing condensation reaction on the acridone acetic acid and substituted pyrimidine in the presence of TCFH and NMI condensing agents to obtain the target compound. The preparation method of the N-methyl-2-(9-oxoacridin-10(9H)-yl)acetamide compound provided in the application is simple and feasible, and good results are shown in in-vitro anti-tumor activity tests, and the compound has excellent anti-proliferation ability on human breast cancer cells BT-549 and MDA-MB-231 in particular.

This invention relates to a 1,1,2,2-tetrahydroperfluoroalkyl-substituted allyl quaternary ammonium salt, its preparation method, and its application, belonging to the field of flocculation treatment technology for high-salt industrial wastewater from natural gas purification. To address the problem that the synthesis of cationic polymer flocculants in existing technologies requires large amounts of surfactants and involves complex operations, this application employs a substitution reaction between 1,1,2,2-tetrahydroperfluoroalkyl iodide and N-methylallylamine; iodomethane is then reacted with the substitution reaction product to undergo quaternization, yielding a 1,1,2,2-tetrahydroperfluoroalkyl-substituted allyl quaternary ammonium salt; the 1,1,2,2-tetrahydroperfluoroalkyl-substituted allyl quaternary ammonium salt is polymerized with acrylamide to obtain a novel cationic polyacrylamide flocculant. The synthesis of cationic fluorocarbon-modified hydrophobic associative polyacrylamide flocculants using an aqueous solution polymerization method is simple, requires no surfactants, and experiments show that the prepared flocculant exhibits excellent flocculation performance.

The invention discloses a synthesis method of a Vinetoram key intermediate and Vinetoram, and relates to the technical field of organic synthesis.The synthesis method comprises the steps that 1-((4 '-chloro-5, 5-dimethyl-3, 4, 5, 6-tetrahydro-[1, 1'-biphenyl]-2-yl) methyl) piperazine hydrochloride and 2-((1H-pyrrolo [2, 3-b] pyridine-5-yl) oxy)-4-bromobenzoic acid methyl ester are used as reaction raw materials, a reaction is carried out, and the Vinetoram key intermediate and the synthesis method of the Vinetoram key intermediate are synthesized; the method comprises the following steps: carrying out a substitution reaction and a hydrolysis reaction to obtain a key intermediate of the Venotocork, and carrying out a condensation reaction on the intermediate and 3-nitro-4-((tetrahydro-2H-pyran-4-yl) methylamino) benzenesulfonamide to obtain the Venotocork. The synthesis method has the advantages of short process route, easily available raw materials, mild reaction conditions, high yield and purity of the intermediate and the Vinetoram, facilitation of the improvement of the yield and quality of the Vinetoram, and reduction of the production cost of the Vinetoram.

The invention discloses a synthesis method of Peniterpheyl A. According to synthesis of a key structural unit furan ring, diphenyl ether is synthesized through a simple heating substitution reaction of a phenol derivative and a fluorobenzene derivative, then C-C direct oxidative coupling of double benzene rings in a molecule is achieved under a Pd / Ag catalytic system to synthesize the furan ring, and due to steric hindrance and guiding group effects, the furan ring can be synthesized into the furan ring. The product has high selectivity, does not need harsh reaction conditions, has simple synthesis steps, is suitable for large-scale production, does not need to widely screen specific strains and fermentation conditions compared with a method for obtaining a low-amount target compound from microbial fermentation separation, is simple and efficient, and can guarantee a large amount of compounds required by subsequent research and development.

The invention relates to a synthesis method of an intermediate for preparing a THR-beta agonist, and belongs to the technical field of medicine synthesis. The synthesis method of the intermediate for preparing the THR-beta agonist is realized by utilizing a substitution reaction of 1H-pyrazolo [4, 3-b] pyridine and 2, 6-dichloro-p-nitrofluorobenzene and a Katada reaction, has the advantages of easiness in large-scale production, controllable quality, controllable cost and the like, and compared with an existing preparation method, the yield of the preparation method disclosed by the invention is greatly improved, and the synthesis method is suitable for industrial production. The raw materials are cheap, easy to obtain, simple and efficient, and have great industrialization prospects.

The application discloses an O-desmethylvenlafaxine prodrug and a preparation method and application thereof, relates to the technical field of drug synthesis, and the structural formula of the O-desmethylvenlafaxine prodrug is shown in the following formula: The phenolic hydroxyl in the structure of the O-desmethylvenlafaxine is etherified or carbonated through a substitution reaction, O-desmethylvenlafaxine prodrug is synthesized, the bioavailability of the O-desmethylvenlafaxine can be remarkably improved, and a compound with the prodrug property is screened through a pharmacokinetics test.

The invention discloses a preparation method of hexa-naphthyloxy cyclotriphosphazene, which comprises the following steps: adding alkali metal hydroxide into a reaction solvent in which naphthol is dissolved, and reacting at 40-60 DEG C for 20-40 minutes to prevent oxygenolysis so as to prepare an alkali metal naphthol salt solution; the solution is stirred and dropwise added into a reaction solvent containing hexachlorocyclotriphosphazene, the ratio of hexachlorocyclotriphosphazene to the solvent is 1: 20-1: 30, the ratio of naphthol to hexachlorocyclotriphosphazene is larger than or equal to 6: 1, substitution is carried out step by step, after dropwise adding is completed, a reaction is carried out for 12-24 h at the temperature of 80-120 DEG C, and six chlorine atoms are completely substituted by naphthyloxy; filtering reaction liquid, and washing a filter cake with a solvent; and carrying out reduced pressure distillation on the filtrate to recover the solvent, washing the crude product with ethanol to remove an intermediate and an oligomer, washing with water to remove water-soluble impurities, filtering, and drying to finally obtain the high-purity hexa-naphthyloxy cyclotriphosphazene with the melting point of 169 DEG C. According to the method, the high-purity hexa-naphthyloxy cyclotriphosphazene crystal is ensured to be obtained by accurately controlling substitution reaction conditions and a multi-stage purification process.

The application discloses a preparation method of a key intermediate of a montelukast sodium side chain acid, belongs to the technical field of pharmaceutical intermediates, and relates to a key intermediate of a montelukast sodium side chain acid, i.e. 1-bromomethylcyclopropylacetonitrile, which is characterized by the preparation method of the 1-bromomethylcyclopropylacetonitrile. The preparation method is as follows: taking tribromoneopentyl alcohol as a starting material, and obtaining 1-bromomethylcyclopropylacetonitrile through a cyclization reaction, an iodination reaction and a cyano substitution reaction. The 1-bromomethylcyclopropylacetonitrile is prepared by using a brand-new synthesis process, starting from tribromoneopentyl alcohol, through a cyclization reaction, an iodination reaction and a cyano substitution reaction. The method solves the blank of the preparation method of 1-bromomethylcyclopropylacetonitrile in the prior art, and also solves the defects of a long reaction theoretical cycle and a low actual yield and a large amount of impurities in the reaction of preparing 1-bromomethylcyclopropylacetonitrile by first preparing 1-hydroxymethylcyclopropylacetonitrile and then reacting phosphorus tribromide with the 1-hydroxymethylcyclopropylacetonitrile.

The application relates to a synthesis method of a phenothiazine derivative, and belongs to the technical field of synthesis in organic chemistry. A diaryl iodonium salt and N-(2-mercapto phenyl)-4-methyl benzene sulfonamide are used as starting materials, and chlorpromazine and perphenazine are obtained through a plurality of steps of substitution reaction, reduction reaction, addition reaction and deprotection reaction. In the application, the reaction raw materials are easy to obtain, the yield is high, and chlorpromazine and perphenazine can be successfully obtained.

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.

The present application relates to the technical field of pesticides, and discloses a chromene aryl hydrazide derivative, a preparation method and application thereof, a structural general formula of the chromene aryl hyydrazide derivative is as formula (I); the preparation method is as follows: taking p-hydroxybenzaldehyde as raw material, and obtaining the chromene aryl hydrazide compound through substitution reaction, cyclization reaction, oxidation reaction, acylation reaction and hydrazinolysis reaction. The chromene aryl hydrazide compound is used for preparing an agricultural bacteriostatic agent. The present application combines aryl hydrazine and chromene skeleton by using the pharmacophore splicing principle in medicinal chemistry, and designs and synthesizes a series of chromene aryl hydrazide compounds. The bacteriostatic activity test result shows that the compounds have excellent bacteriostatic activity, and can be used as active ingredients for preparing a plant pathogenic fungus fungicide.

The application provides a synthesis method of 4-(hydroxymethyl phosphine) 2-carbonyl butyric acid, comprising the following steps: a) mixing acryloyl chloride, a first solvent, a polymerization inhibitor, a catalyst and sodium cyanide, performing a substitution reaction, and obtaining an acryloyl cyanide intermediate after reduced pressure distillation; b) mixing the acryloyl cyanide intermediate obtained in the step a) with hydrochloric acid and a polymerization inhibitor, performing a hydrolysis reaction, and obtaining 2-carbonyl-3-butenoic acid crude product after purification treatment; c) mixing the 2-carbonyl-3-butenoic acid crude product obtained in the step b) with a second solvent and methyl phosphinite, performing an addition reaction, recovering the solvent after water separation and extraction, and obtaining a ketonic acid ester solution; and d) adding hydrochloric acid to the ketonic acid ester solution obtained in the step c) to adjust the pH to be less than or equal to 3, performing a hydrolysis reaction, and obtaining 4-(hydroxymethyl phosphine) 2-carbonyl butyric acid after purification. The synthesis method selects inexpensive acryloyl chloride as a raw material, has mild reaction conditions, is simple to operate, has low production cost, is easy to realize industrialization, and has high yield.