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29 results about "Nitro reduction" patented technology

Synthesis method of 5-(1H-pyrrole-1-yl)-2-mercaptobenzimidazole

The invention discloses a synthesis method of 5-(1H-pyrrole-1-yl)-2-mercaptobenzimidazole, which comprises the following steps: carrying out cyclization condensation reaction on o-phenylenediamine and thiourea in an acidic environment provided by hydrochloric acid to obtain 2-mercaptobenzimidazole; the preparation method comprises the following steps: carrying out nitration reaction on 2-mercaptobenzimidazole, sulfuric acid and nitric acid to obtain 2-mercapto-5-nitrobenzimidazole; the preparation method comprises the following steps: carrying out nitro reduction reaction on 2-sulfydryl-5-nitrobenzimidazole and hydrogen under the catalysis of nickel to obtain 5-amino-2-sulfydryl benzimidazole; the preparation method comprises the following steps: carrying out an N-alkylation reaction on 5-amino-2-mercapto benzimidazole and tetrahydro-2, 5-dimethoxyfuran under the catalysis of copper chloride to generate 5-(1H-pyrrole-1-yl)-2-mercapto benzimidazole, and carrying out a reaction on the 5-amino-2-mercapto benzimidazole and tetrahydro-2, 5-dimethoxyfuran to generate the 5-(1H-pyrrole-1-yl)-2-mercapto benzimidazole. The method disclosed by the invention has the outstanding advantages of mild and easily-controlled conditions, simple and convenient post-treatment, high yield, economy, environmental protection, suitability for large-scale production and the like, conforms to the green chemical development concept, and has important application value.
Owner:ANHUI UNIV

Synthesis method of Olrabatinib

PendingCN121824536AOrganic chemistryAntineoplastic agentsAmine alkylationSilanes
The invention discloses a synthesis method of Olrabatinib, which comprises the following steps: by taking 2-methyl-5-nitro trifluorotoluene as a raw material, carrying out a Waller-Ziegler reaction, an alkylation / silanization reaction of amine, nitro reduction, a condensation reaction and a Caslow-Stevens coupling reaction, so as to obtain the Olrabatinib. By optimizing process conditions and a reaction system, the synthesis method disclosed by the invention has the remarkable advantages in the following aspects: the raw material cost is greatly reduced by adopting low solvent consumption; the product yield is improved by accurately controlling reaction parameters; a standardized post-treatment process is developed, and large-scale stable production is realized. According to the technical system, the technical bottlenecks of high energy consumption and high pollution in the traditional synthesis route are effectively solved, and an innovative solution is provided for green manufacturing of fine chemicals.
Owner:ANHUI UNIV

A synthetic process of (-)-a-lycorane alkaloid

The application discloses a synthesis process of (-)-alpha-lycorane alkaloid and belongs to the technical field of organic synthesis chemistry. (2Z,4E)-7,7-diethoxy-3-hydroxyhepta-2,4-dienoic acid methyl ester and 3,4-methylenedioxy-beta-nitrostyrene are used as starting materials, and (-)-alpha-lycorane is obtained through catalytic asymmetric tandem Michael addition reaction, nitro reduction amination reaction, Boc amidation reaction, Bischler-Napieralski cyclization reaction, ketone enolization tandem esterification reaction, enol triflate reductive hydrogenolysis reaction and amide reduction reaction in sequence. (-)-Alpha-lycorane has a four-membered ring core skeleton of pyrrole-phenanthridine ring, has good in-vitro tumor inhibition activity and cell proliferation growth inhibition activity. The synthesis process can realize efficient, simple and full synthesis of (-)-alpha-lycorane.
Owner:QUJING NORMAL UNIV

A method for synthesizing a tridentate linker fragment useful for improving the hydrophilicity of antibody drug conjugates

The application discloses a synthesis method of a trident connecting segment which can be used for improving hydrophilicity of an antibody drug conjugate, and relates to the field of organic synthesis. The {[5-amino-2-(3,3,4,4-tetramethyl-2-oxa-3-silapent-1-yl)phenyl]methyl}(methyl)amino)methane acid-2-methylpropan-2-yl ester can be used for connecting a hydrophobic dipeptide, a hydrophilic chain and a small molecule drug in an ADC drug, so as to prolong the action time of the ADC drug. The application takes cheap and easily obtained commercial raw material 2-bromo-5-nitrobenzaldehyde as a starting raw material, and successfully prepares the target product through seven steps of conventional transformation such as reduction amination, protection, coupling, ozonation and nitro reduction, with a total yield of about 60% and a scale of hundreds of grams. The starting raw material is cheap, the operation and treatment are simple, and the reaction condition is mild, so that the application is a brand-new process synthesis route, and has good economic benefits and market prospects.
Owner:WUHAN AOFEI TECH CO LTD

A process for the preparation of bumetanide

The application provides a preparation method of bumetanide, taking p-chlorobenzoic acid as a starting material, performing chlorosulfonation, nitration, and ammonolysis to obtain a key intermediate of 3-(N-(tert-butyl) sulfamoyl)-4-chloro-5-nitrobenzoic acid, then performing phenoxylation, nitro reduction, n-butylation, and tert-butyl removal, and finally obtaining the bumetanide. Compared with the synthesis process of the prior art, the method has less side reactions, low cost, high yield, high safety, and is beneficial to industrial production.
Owner:SUZHOU INST OF MATERIA MEDICA CHINA SCI & TECH

Preparation method and application of N-alkylamide natural product Cubebamide and analogue thereof

The invention relates to a preparation method and application of an N-alkyl amide natural product Cubebamide and an analogue thereof, and belongs to the field of compound technologies and medicinal chemistry. According to the invention, commercially available 3, 4, 5-trimethoxybenzaldehyde 1 is used as a raw material, a compound 3 is obtained through a Horner-Wadsworth-Emmons (HWE) reaction, and then a compound 4 is obtained through hydrolysis. A compound 5a-5f is used as a raw material, a compound 6a-6f is synthesized through a Henry reaction, and a compound 8a-8f is obtained through double bond and nitro reduction. And carrying out condensation reaction on the two fragments 4 and 8a-8f to obtain the natural product Cubebamide and the analogue 9a-9f thereof. The compounds 9a, 9c and 9d disclosed by the invention have relatively good anti-inflammatory activity; the compounds 9b, 9e and 9f have remarkable anti-inflammatory activity. The synthesis method has the advantages of easily available raw materials, mild reaction conditions, environmental protection and simple operation.
Owner:CHENGDU UNIV

Preparation method of hydrogen-containing silane mediated benzoxazole derivative

The invention relates to the technical field of organic synthesis, in particular to a preparation method of hydrogen-containing silane mediated benzoxazole derivatives, which comprises the following steps: (2-nitrophenyl) benzoate and analogues thereof as nitro substrates are dissolved in acid liquor with a palladium catalyst, hydrogen-containing silane is slowly injected, reaction is carried out under normal pressure, after the reaction is finished, a reaction product is subjected to post-treatment, and the hydrogen-containing silane mediated benzoxazole derivatives are obtained. Separating and purifying to obtain a target product benzoxazole derivative. The novel synthesis method of benzoxazole and derivatives thereof is adopted, high-pressure hydrogen and inert gas protection required by a traditional hydrogenation method is abandoned, nitro reduction and cyclization are completed in one step, and a safe, economical and environment-compatible synthesis scheme is provided for large-scale production of benzo-azacyclo drug intermediates.
Owner:ZHEJIANG UNIV OF SCI & TECH

Omariglonide intermediate, preparation method thereof and method for preparing key intermediate of Omariglonide

The invention provides an omariglitazone intermediate, a preparation method thereof and a method for preparing an omariglitazone key intermediate, and relates to the technical field of organic chemistry. The omarignelone intermediate provided by the invention has a structure as shown in a formula VIII; the omariglitazone intermediate is easy to obtain and can be conveniently prepared by taking benzaldehyde as a starting raw material, a chiral chromatographic column does not need to be used for preparation of the omariglitazone intermediate, a key chiral center of the omariglitazone intermediate is constructed by catalyzing a cheap chiral amine catalyst through an asymmetric Knoevenagel-Michael addition reaction, and the preparation method is simple and convenient. According to the omariglitazone intermediate, industrial production of the omariglitazone key intermediate (the structure as shown in the formula I) is easy to realize, and the production cost is reduced. The invention provides a method for preparing an omariglone key intermediate (a structure shown in a formula I), the omariglone key intermediate can be prepared from the omariglone intermediate through a nitro reduction reaction, a Jappp-Klingemann reaction and an indole synthesis reaction, and the method is suitable for industrial production. A formula VIII and a formula I are shown in the description.
Owner:JIANGXI SYNERGY PHARMA

A process for the preparation of 2-acetylamino-4-[(2-hydroxyethyl)sulfonyl]benzoic acid

The application discloses a preparation method of 2-acetylamino-4-[(2-hydroxyethyl)sulfonyl]benzoic acid. The 2-acetylamino-4-[(2-hydroxyethyl)sulfonyl]benzoic acid is prepared from 4-fluoro-2-nitrobenzoic acid methyl ester as a starting material through aromatic nucleophilic substitution reaction, nitro reduction reaction, ester hydrolysis reaction, amino acylation reaction, thioether oxidation reaction and the like. The method has the advantages of mild reaction condition, high yield, low cost, easy availability of raw materials, and the like. The synthesis process meets the requirements of green chemistry, the synthesis route is innovative, the reaction post-treatment is simple, and the product is easy to purify.
Owner:ANHUI UNIV

The method comprises the following steps: synthesizing 4, 4 apos from p-nitrobenzoyl chloride; process for preparing-difluorobenzophenone

The invention provides a method for synthesizing 4, 4 '-difluorobenzophenone from p-nitrobenzoyl chloride, and belongs to the field of organic synthesis. The method comprises the following steps: (1) reacting paranitrobenzoyl chloride with aromatic fluoride in the presence of a catalyst to obtain 4-nitro-4 '-fluorobenzophenone; (2) carrying out nitro reduction reaction on the 4-nitro-4 '-fluorobenzophenone obtained in the step (1) to obtain 4-amino-4'-fluorobenzophenone; and (3) carrying out diazotization reaction on the 4-amino-4 '-fluorobenzophenone obtained in the step (2), anhydrous hydrogen fluoride and sodium nitrite, and after the reaction is finished, heating and carrying out cracking reaction to obtain the product 4, 4'-difluorobenzophenone. In the synthesis process, the generation of isomers is avoided, the reaction selectivity is improved, the generation of 4-fluorobenzophenone impurities is reduced, the product purity is improved, and a guarantee is provided for the quality of downstream polyether-ether-ketone products.
Owner:JILIN ZHONGYAN HIGH PERFORMANCE PLASTIC CO LTD

Synthesis method of camptothecin derivative

PendingCN121991087AAvoid yield decayhigh yieldOrganic chemistryMannich reactionKetone
The present invention relates to the technical field of camptothecin derivative preparation, particularly to a camptothecin derivative synthesis method, which uses 2-nitroacetophenone and isopropylamine as raw materials, and the camptothecin derivative is obtained through a Mannich reaction, a methylsulfonylation reaction, a nitro reduction reaction and a ring closing reaction. According to the synthetic method of the camptothecin derivative, the complex camptothecin derivative is split into two segments 1-(2-aminophenyl)-3-(N-isopropyl-N-methylsulfonylamino) propan-1-one and a compound V which are easy to prepare, and finally, a plurality of rings and chemical bonds are constructed simultaneously through one-step efficient ring closing reaction. The yield attenuation caused by progressive multiplication of the yield in the traditional linear synthesis is avoided, and the total yield is improved.
Owner:DEYANG YUEHE BIOMEDICAL TECHNOLOGY CO LTD

High-dispersion metal co-doped carbon catalyst as well as preparation method and application thereof

The invention discloses a high-dispersion metal co-doped carbon catalyst and a preparation method and application thereof.The preparation method comprises the steps that S1, organic matter is adsorbed by layered double-metal hydroxide, and organic-carbon-containing micromolecule anchored layered double-metal hydroxide is obtained; and S2, carrying out heat treatment on the micromolecular anchoring layered double metal hydroxide containing the organic carbon at the temperature of 600-1400 DEG C. The catalyst is prepared by the method and can be used for catalyzing nitro reduction reaction of aromatic hydrocarbon. The high-dispersion metal co-doped carbon catalyst prepared by the invention has very high catalytic activity, stability and cycle performance, can realize magnetic separation, and is especially suitable for catalysis of reduction reaction of aromatic nitro compounds. The preparation method has the advantages of cheap and easily available raw materials and simple process, and is suitable for large-scale industrial production.
Owner:HUNAN RES INST FOR NONFERROUS METALS CO LTD

Polyimides containing dibenzofuran / dibenzothiophene and triphenylamine structures, and methods of making and using the same

PendingCN122444992APolymer scienceAniline
Polyimide containing dibenzofuran (thiophene) and triphenylamine structure and preparation method and application thereof, and application thereof, the present application relates to polyimide containing dibenzofuran (thiophene) and triphenylamine structure and preparation method and application thereof. In order to solve the problem of low solubility of aromatic polyimide in organic solvent, poor optical contrast, slow response time and poor capacitor performance, 2,8-dibromodibenzofuran (thiophene) is used as raw material, and 4-methoxy-4'-nitrodiphenylamine is reacted to obtain a new precursor containing dibenzofuran (thiophene) and triphenylamine structure. The nitro group is reduced to obtain a diamine monomer, which is polymerized with dianhydride to form a new high-performance polyimide. At the same time, the polymer has excellent electrochromic performance, including excellent cycle stability, fast switching time, high optical contrast and low voltage start. It also has excellent capacitor performance, including excellent specific capacity and cycle stability. The present application is expected to be applied in the field of electrochromic supercapacitor.
Owner:HEILONGJIANG UNIV

A method for synthesizing milobalin benzylsulfonic acid

ActiveCN117886708BCyclobutaneNitromethane
This invention provides a method for synthesizing milobalin benzylsulfonic acid, comprising the following steps: a chiral enone undergoes a condensation reaction with cyanoacetate in the presence of ammonium acetate to obtain an unsaturated cyano ester; next, the unsaturated cyano ester undergoes a condensation reaction with nitromethane to obtain a nitro ester; the nitro ester is then deesterified at high temperature to obtain a chiral nitro nitrile, which is then reduced to a chiral amino nitrile; subsequently, the chiral amino nitrile is hydrolyzed to obtain the free base of milobalin; finally, the free base of milobalin is salted with benzylsulfonic acid to obtain milobalin benzylsulfonic acid. This invention stereospecifically constructs a chiral cyclobutane quaternary carbon center to obtain a chiral nitro ester with a single stereoconfiguration, avoiding the chiral isomer waste generated by chiral isomer resolution, eliminating the need for chiral column separation or chiral resolution, significantly reducing production costs, and simultaneously avoiding the environmental pollution caused by residual heavy metal titanium in the product and solid waste heavy metal titanium.
Owner:ZHEJIANG TIANYU PHARMA +1

Synthetic method of 6-bromoindole-2-carboxylic acid

The invention relates to the field of chemical synthesis, in particular to a synthesis method of 6-bromoindole-2-carboxylic acid. Comprising the following steps: preparing 4-bromo-2-aminotoluene; preparation of 6-bromoindole-2-carboxylic acid ethyl ester; and preparing the 6-bromoindole-2-carboxylic acid. According to the present invention, the reduction cyclization and hydrolysis process is improved, the diethyl malonate is adopted as the mild reducing agent, and the step-by-step temperature control technology is combined so as to significantly improve the yield and the purity; the invention discloses a three-step synthesis process of a bromo-indole carboxylic acid derivative. The method comprises the following steps: 1, in an improved mixed solvent system, carrying out a reduction reaction of reducing nitryl into amino; in the second step, a controllable reduction cyclization technology is adopted, and nitro amination is achieved; in the third step, the ester bond breaking efficiency is improved through the synergistic effect of alkaline hydrolysis and a solvent.
Owner:JINING SHENGTAI PHARM CO LTD

Low-temperature orientation agent material

The invention relates to the technical field of orientation agents, in particular to a low-temperature orientation agent material. The low-temperature orientation agent material is prepared by the following steps: performing Suzuki coupling reaction on 4-broronitrobenzene and 4-perfluorohexyl butyl boric acid to prepare an intermediate A, performing nitro reduction to obtain an intermediate B, and finally performing ureation reaction on the intermediate B and isocyanate ethyl acrylate to obtain the low-temperature orientation agent material. The low-temperature orientation agent can be used for preparing a constant-transparent mode dimming film; the normally transparent mode dimming film is prepared by coating a composition containing a microcrystal composition, a polymerizable composition, a photoinitiator and the orientation agent between two layers of PET-ITO conductive films and carrying out ultraviolet curing and other processes, and the middle layer is a vertical orientation polymer microcrystal layer. A traditional PI layer technology is not needed, the production process is simplified, the orientation agent can still stably anchor and induce orientation at low temperature, the dimming performance and durability of the dimming film can be improved, and the application range of the dimming film in a low-temperature scene is effectively widened.
Owner:SHANGHAI ASTRACE NEW MATERIAL TECH CO LTD

Production system and production method of medicinal p-aminobenzoic acid

The invention discloses a production system and a production method of medicinal p-aminobenzoic acid. The production system comprises a filter column, a hydrogenation reaction kettle, a catalyst filter, a tubular hydrogenation reactor, a fine filter and a crystallization kettle, the production method comprises the following steps: pumping p-nitrobenzoic acid and a solvent into a hydrogenation reaction kettle through a filter column, and reacting until 3-5% of raw materials are left; then pressing out the material from the hydrogenation reaction kettle, enabling the material to enter a tubular hydrogenation reactor through a catalyst filter for continuous reaction until the material is completely reacted, finally filtering the liquid material through a micro-filter, and enabling the liquid material to enter a crystallization kettle for crystallization. On one hand, a small amount of residual colored impurities, heavy metal impurities and insoluble tiny foreign matters in raw materials are removed by adopting a multi-effect filter column, and on the other hand, hydrogenation reaction is carried out by adopting a manner of connecting a kettle type reactor and a tubular reactor in series; the content of intermediate-state impurities in nitro reduction and the content of impurities in side reactions such as decarboxylation and polymerization can be effectively reduced, and finally para aminobenzoic acid meeting the medicinal-grade requirement can be obtained.
Owner:CHANGZHOU SUNLIGHT PHARMA

A method of photo-initiated nitro-reduction hydrogenation

The application discloses a method for photo-induced nitro reduction hydrogenation, and belongs to the field of medical compound synthesis.The method provided by the application takes iron trichloride and palladium-carbon as the catalysts of main reactions, and realizes nitro reduction into amino under the conditions of normal temperature, normal pressure and nitrogen, the reaction has high catalytic efficiency and fast reaction rate, the reaction time is only 10 minutes, the yield of the product obtained by nitro reduction is high, the experimental cost is greatly reduced, the method is suitable for the synthesis and amplification of later-stage compounds, the method has simple steps, wide substrate application range, and the effects of high efficiency, green environmental protection, safety and cost saving, and the reaction has fast reaction rate, and has excellent application prospect in industrial production.
Owner:SHANDONG FIRST MEDICAL UNIV & SHANDONG ACADEMY OF MEDICAL SCI

A process for the preparation of N-(3-bromo-5-fluoro-4-methylphenyl)acetamide

The application belongs to the technical field of biological medicine, and particularly relates to a preparation method of N-(3-bromo-5-fluoro-4-methylphenyl)acetamide. The application takes 3,4-difluoro-5-bromonitrobenzene as an initial raw material, first carries out a coupling reaction with malonic acid diethyl ester, then carries out a decarboxylation reaction in the presence of a chlorinated salt, then carries out a nitro reduction reaction in the presence of a reducing agent and a catalyst, and finally carries out amino protection by using acetic anhydride. The preparation method provided by the application obtains the target product N-(3-bromo-5-fluoro-4-methylphenyl)acetamide through four-step reactions, has high total yield of the target product, is simple to operate, has good repeatability, has few side reactions, is simple to purify, has low production cost, and is suitable for industrialized scale production. As shown in the test results of examples, the total yield of N-(3-bromo-5-fluoro-4-methylphenyl)acetamide prepared by the preparation method provided by the application is 78.4%.
Owner:ACCELA CHEMBIO CO LTD

Photoresist for capacitive touch sensor and preparation process thereof

The invention relates to the technical field of photoresist, in particular to photoresist for a capacitive touch sensor and a preparation process of the photoresist. The invention discloses a preparation process of photoresist for a capacitive touch sensor. The preparation process comprises the following steps: preparing a modified photoreaction agent; preparing modified polyimide resin powder; preparing silicon dioxide hollow carbon spheres and nano titanium dioxide hybrid particles; and preparing the photoresist. The preparation method comprises the following steps: firstly carrying out nitration reaction on 4-tert-butylphenol, then reducing nitryl into amino to obtain amino substituted 4-tert-butylphenol, protecting the amino by di-tert-butyl dicarbonate ester, then oxidizing iodobenzene into a high-valence iodine active intermediate by taking m-chloroperoxybenzoic acid as an oxidizing agent, and reacting with Boc-amino substituted 4-tert-butylphenol to obtain the high-valence iodine-substituted 4-tert-butylphenol. And finally, carrying out a replacement reaction with silver trifluoromethanesulfonate, carrying out deprotection to obtain a modified photoreaction agent, and carrying out a condensation polymerization reaction on the modified photoreaction agent, 4, 4 '-hexafluoroisopropyl phthalic anhydride and the like to generate a polyamic acid prepolymer, so that the photoetching resolution can be greatly improved.
Owner:江苏佳合盛科技有限公司

Porphyrin-based COFs photocatalyst, preparation method thereof and application of porphyrin-based COFs photocatalyst in photocatalytic production of H2O2

The invention discloses a porphyrinyl COFs photocatalyst, a preparation method and application in photocatalytic production of H2O2, and belongs to the technical field of material scientificity, firstly 5, 10, 15, 20-tetra (tetranitrophenyl) porphyrin is synthesized, then nitro on the porphyrin is reduced into amino, then 4, 4 '-(10-(9-anthryl)-5, 5-difluoro-3, 7-dimethyl-5H-4, 5-dipyrrolo [1, 2-c: 2', 1 '-f] [1, 3, 4] triazolo [1, 2-c: 2', 1 '-f] [1, 3, 4] triazolo [1, 3, 4] triazolo [1, 3, 4] triazolo [1, 3, 4] triazolo [1, 3, 4] triazolo 2, 2] (2, 8-diazoboron pyridinyl) dibenzaldehyde is prepared, the two monomers are dispersed in an organic solvent, and solvothermal polymerization is performed under the catalysis of anhydrous acetic acid to form the COF material. Porphyrin has a large conjugate structure of 18 pi electrons and has excellent visible light absorption capability and electron donating characteristic, and the large conjugate structure provides stable nodes for constructing a COF topological structure. In combination with the characteristics of high charge transfer rate, large specific surface area and high visible light utilization efficiency of the COF material, the prepared COFs have higher charge separation capacity and have the capacity of absorbing the whole visible light range. The synthesis process is simple, and an effective way is expected to be provided for producing H2O2 through efficient photocatalysis of the COF material.
Owner:SHAANXI UNIV OF SCI & TECH

A method for preparing nano-sized ammoniated aramid fibers by nitration followed by reduction with mixed acids

This invention discloses a method for preparing nano-sized ammoniated aramid by nitration followed by reduction in mixed acid, belonging to the fields of chemistry and materials technology. This invention uses waste aramid as raw material, utilizing the nitryl ions in mixed acid to convert aramid into nitrated aramid; then, using a relatively inexpensive tin dichloride catalyst under mild conditions, the nitro groups on the nitrated aramid are reduced to amino groups, successfully preparing ammoniated aramid. The method for preparing nano-sized ammoniated aramid by nitration followed by reduction in mixed acid has the following advantages: (1) simple operation, low cost, and conducive to industrial production; (2) low reaction temperature, mild experimental conditions, and sustainability; (3) fast reaction and short cycle; (4) convenient product collection, facilitating subsequent use.
Owner:NORTHEASTERN UNIV CHINA

A fluorine-containing bromoaniline compound and a preparation method thereof

This invention discloses a fluorobromoaniline compound and its preparation method, belonging to the field of organic synthesis technology. The method employs a three-step synthetic pathway starting with 2,6-difluoronitrobenzene, involving sequential ammonolysis, diazotization bromination, and nitro reduction. Utilizing the triple function of the nitro group: firstly, it acts as a strong electron-withdrawing group, guiding the ammonolysis reaction selectively at the fluorine atom at the 6-position, generating 2-fluoro-3-nitrobenzene; subsequently, the diazotization step stabilizes the diazonium salt intermediate, ensuring the specific substitution of the bromine atom at the original amino position, yielding 2-fluoro-6-bromonitrobenzene; finally, the nitro group is gently reduced to the amino group to obtain the target product. This invention eliminates the need for amino protection and deprotection steps, avoiding the use of precious metal catalysts and hazardous reagents. It possesses advantages such as high regioselectivity, high atom economy, and a simple procedure, making it suitable for continuous industrial production and providing a novel approach for the efficient preparation of pharmaceutical and material intermediates.
Owner:FUXIN JINHONGTAI CHEM

Synthesis of pyrrolo[1,2-a]quinoxaline compounds from nitro-pyrroloarene and carbon dioxide and a method thereof

The application discloses a kind of nitryl pyrrole arene and carbon dioxide synthesis pyrrolo [1, 2-a] quinoxaline compound and synthesis method thereof, using simple and easy nitryl pyrrole arene and carbon dioxide as raw material, under the mediation of cheap and easy polymethyl hydrogen siloxane, using efficient catalytic system, it is first reduced to amino that nitryl, subsequently again with polymethyl hydrogen siloxane capture carbon dioxide after the reaction of silicon ester generated, and then intramolecular electrophilic cyclization is obtained target product.The method is simple, one pot realizes reduction and cyclization multi-step reaction, step economy is efficient and target compound is rich in variety.In addition, the substrate of the method of the application is better in universality, under the optimized reaction condition, target product is easy to separate, has potential application value in material and pharmaceutical field.
Owner:SHAANXI UNIV OF SCI & TECH

A method for synthesizing a dipyridamole key intermediate

The application discloses a synthesis method of a dipyridamole key intermediate. The synthesis method of the dipyridamole key intermediate comprises the following steps: condensing ethyl 2-nitroacetate with ethyl oxalate, then condensing with urea, reducing the nitro group, condensing with urea again, chlorinating, and finally condensing with piperidine, so as to obtain the dipyridamole key intermediate 2,6-di-chloro-4,8-dipiperidyl-pyrimido[5,4-d]pyrimidine. The method avoids traditional nitrification and nitric acid oxidation processes, and the whole process is free of dangerous process, the reaction condition is mild, and the product yield is high.
Owner:NANTONG SENXUAN PHARM CO LTD

Nitro reduction reaction based on droplet acceleration

The invention discloses a nitro reduction reaction based on liquid drop acceleration. According to the invention, the liquid drop chemistry is proposed for the first time to accelerate the reduction of nitryl to amido, and mild and efficient synthesis of organic amine compounds, especially aromatic amines such as paracetamol and the like can be realized; moreover, on the basis of a cascade reaction of liquid drop accelerated nitro reduction and Cartesian condensation, the invention also provides an on-line derivative nitro compound to be an ionic pyridinium compound, so that high-sensitivity detection of the nitro compound by the atmospheric pressure mass spectrum is realized, and the bottleneck that the nitro compound cannot be measured by the atmospheric pressure mass spectrum is solved; the method provided by the invention not only provides an efficient and green methodology for synthesis of organic amine drugs, but also provides a method support for high-sensitivity mass spectrum determination of nitro compounds in various samples.
Owner:HANGZHOU NORMAL UNIVERSITY

Continuous flow synthesis method of 4, 6-diamino resorcinol salt

The invention provides a continuous flow synthesis method of 4, 6-diamino resorcinol salt, and belongs to the technical field of chemical synthesis. According to the method, the 4, 6-diamino resorcinol salt is synthesized by automatic control through a continuous flow synthesis route of acetyl protection of phenolic hydroxyl group, nitration, nitro reduction and deacetylation-acidification, the whole reaction process is carried out in a closed environment, the reaction safety and the reaction efficiency are improved, and the method is suitable for industrial production. According to the present invention, the conditions such as the use amount of each reactant, the pumping speed, the reaction time, the reaction temperature and the like are controlled, such that the synthesized 4, 6-diamino resorcinol salt has high purity and high yield, the purity and the yield of the product can respectively achieve 99.9% and 85.0%, and the wide application prospect in the continuous fluidization industrial production is provided.
Owner:ASTATECH (CHENGDU) BIOPHARM CORP +1

A method of synthesizing relugolix

ActiveCN117327091BOrganic chemistryNitro reductionHydrolysis
The application provides a synthesis method of relugolix, comprising the following steps: reacting compound 2 with di-tert-butyl dicarbonate to obtain compound 3; reacting compound 3 with dibromohydantoin to obtain compound 4; reacting compound 4 with dimethylamine hydrochloride to obtain compound 5; hydrolyzing compound 5 to obtain compound 6; condensing compound 6 with 6-methoxy-3-aminopyridazine to obtain compound 7; deprotecting the amino group of compound 7 to obtain compound 8; performing reductive amination on compound 8 with 2,6-difluorobenzaldehyde to obtain compound 9; performing nitro reduction on compound 9 to obtain compound 10; and reacting compound 10 in the presence of carbonyldiimidazole and methoxyamine hydrochloride to obtain relugolix. The synthesis method is more efficient than prior art, avoids potential genotoxic impurities in the prior art, has mild process conditions, high reaction yield in each step, effectively reduces industrial production cost and safety risk, and is suitable for industrial production.
Owner:ZHEJIANG TIANYU PHARMA