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68results about How to "Avoid harsh reaction conditions" patented technology
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Synthesis method of 2, 5-disubstituted thiophene compound
ActiveCN102115468AWide variety of sourcesSimple and fast operationOrganic active ingredientsSaccharide with carbocyclic radicalsState of artReaction conditions
Owner:TOPHARMAN SHANDONG
Imine alkali metal salt and ion liquid and application of same as non water electrolyte
InactiveCN102816096AEasy to separate and purifyHigh yieldAmino preparation from aminesCarboxylic acid nitrile preparationCation compositionAlkali metal
The invention provides ion liquid composed of fluoroalkyl sulfimide salt alkali metal salt containing 'S-fluoroalkyl sulfimide group', fluoroalkyl sulfimide negative ions containing 'S-fluoroalkyl sulfimide group' and positive ions of sulfonium salt, ammonium salt and microcosmic salt. The ion liquid utilizes (fluoroalkyl sulfonyl) (fluoroalkyl sulfinyl) imine with sulfur valence state as +4 and hydroxylamine oxygen sulfonic acid to react to prepare intermediate fluoro alkyl (S- fluoroalkyl sulfimide group) sulfamide of fluoroalkyl sulfimide, effectively shortens the line that the (fluoroalkyl sulfonyl) (fluoroalkyl sulfinyl) imine is utilized to prepare fluoro alkyl (S- fluoroalkyl sulfimide group) sulfamide of fluoroalkyl sulfimide through the three steps of chlorination, fluorination and amination, and is convenient to operate and high in yield and purity. The alkali metal salt has good heat stability and hydrolysis resistance, has high conductivity and oxidation potential in traditional carbonic ester solution, and is good in compatibility with electrode materials widely used. The ion liquid can be applied to lithium ion batteries and carbon-based super capacitors.
Owner:HUAZHONG UNIV OF SCI & TECH +1
Method for preparing nano diamonds by using direct-current arc process
InactiveCN103482623AAvoid reaction conditionsSimple processMaterial nanotechnologyDiamondCarbon sourceCondensation process
The invention discloses a method for preparing nano diamonds by using a direct-current arc process, belonging to the technical field of preparation of carbon-related nano materials. The method is characterized in that direct-current arc hydrogen plasma is used as a heat source, graphite is used as a carbon source, nickel is used as a catalyst and silicon is used as a nucleation substance to synthesize diamond nano-particles. High-temperature hydrogen plasma is used for evaporating a block composite target material to form atomic and ionic states of raw material components, a silicon carbide cluster crystal nucleus is formed and atoms are induced to form a diamond phase during condensation, carbon atoms separated out from a supersaturated nickel-carbon solid solution become growth substances for the diamond phase, and a nano diamond blank is obtained through passivation. The remaining impurities including metals, graphite, amorphous carbon, silicon carbide and the like are removed through purification processes including acid treatment, high-temperature oxidation, rinsing and the like so as to obtain high-purity diamond nano-particles. The method disclosed by the invention has the effects and benefits that the preparation process is simple, the synthesis is performed under a normal pressure condition, and the low cost, low energy consumption and large-scale production of the diamond nano-particles are realized.
Owner:DALIAN UNIV OF TECH
Method for preparing metal nanomaterial with simulated cell structure
The invention discloses a method for preparing a metal nanomaterial with a simulated cell structure, which is characterized by comprising the following steps of: reducing metal ions in an external metal salt solution on surfaces of metal nanoparticles by using a reducing agent for forming a core-shell structure to form a binary metal core-shell structure; reducing high-valence metal ions in a subsequently added metal salt solution into middle and low-valence metal ions on the surface of the binary metal core-shell structure by using a reducing agent for forming the simulated cell structure; and sacrificing a metal shell through displacement reaction between two kinds of metal to form a simulated cell metal nanostructure consisting of a metal core, a cavity and metal walls. The severe condition required by the conventional single high-temperature metal displacement reaction is avoided, the shape of the original nanometal core can be completely kept, and the nanometal material of which the inner cavity contains the movable metal core is formed; and the metal nanomaterial can be applied to fields of environment detection, industrial catalysis, biomedicine and the like and is high in universality, and the preparation method is simple.
Owner:HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
Synthesis method for industrial production of octreotide
ActiveCN106543269AAvoid harsh reaction conditionsMild reaction conditionsPeptide preparation methodsWater bathsSynthesis methods
The invention relates to synthesis method for industrial production of octreotide. The method is characterized by comprising the following steps of: 1. taking aminomethyl resin as the starting resin, utilizing condensation reagents HOBT and DIC to couple the raw material Fmoc-Thr-x to the resin to generate Fmoc-Thr-x AM Resin; then coupling amino acids Cys, Thr, Lys, Trp, Phe, Cys and Phe to Fmoc-Thr-x AM Resin one by one in order, thus obtaining octreotide peptide resin; 2. adding a lysate solution, stirring the substances evenly and performing cracking for 2-3h; 3. dissolving octreotide crude peptide into a TFA / water mixed solution, then putting the mixture into 35DEG C-38DEG C water bath to perform heating for 2-3h to make the linear peptide of octreotide have single peak pattern in HP LC chromatogram; and 4. adding DMSO, then performing oxidation for 1-1.5h, conducting HPLC detection of a cyclization end point, and performing separation and purification to obtain a refined product of octreotide. In short, the synthesis method provided by the invention has simple technique, and is suitable for industrial production. After post-treatment, the HPLC peak pattern of octreotide crude peptide is simple, the cyclization method is easy to operate, cyclization is complete, the yield is high and the purity is 98% or more.
Owner:苏州天马医药集团天吉生物制药有限公司
Module compound with hydrogen bond sequence specificity combination and preparation method thereof
The present invention discloses a module compound with hydrogen bond sequence specificity combination and a preparation method thereof. The structure formula of the compound module is as follows: wherein, when R is (m is any integer of 1-200), the module compound is a hydrophilic module compound P2; when R is (n is any integer of 2-140), the module compound corresponds to the hydrophobic module compound of BLOCK-1, BLOCK-2 or BLOCK-3. As the module compound has hydrogen-sequence specificity and the two complementary single-stranded can mutually recognize and match with specificity, the block copolymer which is not easy to synthesize by other methods can be easily prepared by using a molecular glue group.
Owner:SHANGHAI JIAO TONG UNIV +1
Synthesis method of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride
InactiveCN104086545ASave raw materialsAvoid reaction conditionsOrganic chemistryHydrogen chlorideAmmonium chloride mixture
The invention relates to a synthesis method of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride, which comprises the following steps: reacting a compound (3) and fluorobenzyl bromide in the presence of DMF (N,N-dimethylformamide) and potassium carbonate to obtain a compound (4); dissolving the compound (4) in absolute methanol, adding sodium methoxide, stirring and reacting to obtain a solution containing a compound (5); and reacting the solution containing the compound (5) with ammonium chloride and glacial acetic acid, and salifying with hydrogen chloride. The synthesis method provided by the invention has the advantages of cheap raw materials, mild reaction conditions and high total yield, is simple to operate, and is suitable for large-scale synthesis of the important intermediate 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride of riociguat for treating adult chronic thromboembolic pulmonary hypertension (CTEPH) and pulmonary artery hypertension (PAH).
![Synthesis method of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride](https://images-eureka.patsnap.com/patent_img/0a889063-b691-47b6-b2e4-65d760c99a65/142113DEST_PATH_IMAGE010.PNG "Synthesis method of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride")
![Synthesis method of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride](https://images-eureka.patsnap.com/patent_img/0a889063-b691-47b6-b2e4-65d760c99a65/15205DEST_PATH_IMAGE002.PNG "Synthesis method of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride")
![Synthesis method of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride](https://images-eureka.patsnap.com/patent_img/0a889063-b691-47b6-b2e4-65d760c99a65/168286DEST_PATH_IMAGE008.PNG "Synthesis method of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride")
Owner:安徽联创生物医药股份有限公司
Biological synthesis method of xylosic acid
InactiveCN103865959AGood product specificityAvoid reaction conditionsBacteriaMicroorganism based processesXyloseInducer
The invention discloses a method for synthesis of xylosic acid by biological catalysis of D-xylose. The method comprises the following steps: A) constructing a recombinant engineering receptor bacteria strain which is capable of converting the D-xylose to the xylosic acid and contains a xylose dehydrogenase gene xylB gene fragment and a xylose acid lactonase gene xylC gene fragment; and B), using the engineering receptor bacteria in the A for fermentation cultivation in a D-xylose-containing culture medium, using an appropriate inducer for introduction, and separating and purifying to obtain the xylose acid.
Owner:QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
Method for high-selectivity preparation of gamma-GVL by homogeneous catalysis
The invention relates to a method for preparing gamma-GVL by homogeneous catalysis. According to the method, levulinic acid esters are taken as raw materials, secondary alcohols are taken as hydrogen sources and solvents, and in the catalysis of aluminium isopropoxide, hydrogen transfer and lactonization are carried out to obtain the gamma-GVL. The method for the high-selectivity preparation of the gamma-GVL by the homogeneous catalysis has the advantages of short reaction time, fast substrate conversion, high conversion rate, high product selectivity and almost no side reaction. The method does not require high-pressure hydrogen in the reaction process, thereby not needing to isolate air; used catalysts are non-noble metal catalysts, so that the prices are low; harsh reaction conditions of requirements on high temperature and high pressure, protection of inert gases and use of noble metal catalysts are avoided in the existing preparation process, and the method disclosed by the invention is mild in reaction conditions, low in equipment requirements, simple in process and convenient to operate. The secondary alcohols in the method can be recycled. The safety and economy of the preparation method are improved.
Owner:CHINA AGRI UNIV
Bifunctional 4-TMS-5-I-1,2,3-triazole compound as well as preparation method and application thereof
InactiveCN104592281AWide variety of sourcesEasy to makeGroup 4/14 element organic compoundsPtru catalystIodide
The invention discloses a bifunctional 4-TMS-5-I-1,2,3-triazole compound as well as a preparation method and application thereof. According to the technical scheme, the bifunctional 4-TMS-5-I-1,2,3-triazole compound is characterized by being prepared at normal temperature, wherein trimethyl silyl acetylene and nitrine serve as raw materials, acetonitrile serves as a solvent, cuprous iodide serves as a catalyst, N-chlorosuccinimide serve as an oxidant, and N-di(isopropyl)ethylamine serves as an alkali. The bifunctional 4-TMS-5-I-1,2,3-triazole compound has a structural formula as shown in the specification, wherein R is as shown in the specification. The invention further discloses a preparation method of the bifunctional 4-TMS-5-I-1,2,3-triazole compound and a method of further synthesizing a 1,5-di-substituted-1,2,3-triazole compound from the bifunctional 4-TMS-5-I-1,2,3-triazole compound which serves as an intermediate. The raw materials are wide in source, are easy to prepare and are low in cost, and the cuprous iodide adopted by reaction serves as the catalyst and the reactant, is very low in cost, is simple and is easy to obtain.
Owner:HENAN NORMAL UNIV
Linear tin phosphide compound and preparation method thereof
The invention discloses a linear tin phosphide compound. A chemical formula of the linear tin phosphide compound is Sn4P3; the linear tin phosphide compound has a linear shape and has the length of 0.1mu m to 12mu m and the length-width ratio is 1 to (1.82 to 35.7). The linear tin phosphide compound is prepared by adopting the following steps: carrying out high-energy ball milling on red phosphorus, tin powder and aluminum powder; carrying out calcination on the obtained powder in a vacuum tubular furnace to obtain the linear tin phosphide compound. According to a preparation method of the linear tin phosphide compound, disclosed by the invention, the production cost is reduced, a generation procedure is greatly simplified, the production time is shortened and the yield is improved. Meanwhile, harsh reaction conditions including a toxic phosphorus source, high pressure and the like are also avoided. A prepared phosphide has a linear structure so that the specific surface area is greatly improved, hydrodesulfurization (HDS), hydrodenitrogenation (HDN) and hydrodeoxygenation (HDO) activity and photocatalysis performance of the phosphide are improved and application performance of the phosphide in a lithium-ion battery material is improved.
Owner:UNIV OF JINAN
Preparation method of 1,2,3-bis-triazole ligands and application of 1,2,3-bis-triazole ligands in CuAAC reaction
ActiveCN105968116AObvious categoryExpand categoryEsterified saccharide compoundsSugar derivativesBis triazoleGlycine methyl ester hydrochloride
The invention discloses a preparation method of 1,2,3-bis-triazole ligands and an application of the 1,2,3-bis-triazole ligands in a CuAAC reaction. With cheap and easily available glycine methyl ester hydrochloride as a base raw material, and through derivation and conversion of functional groups, a diyne compound with glycine as a structure is obtained; then under a condition of room temperature and with organic azide as a raw material and copper iodide as a catalyst, 1,2,3-bis-triazole seven-membered-ring compounds are synthesized; and with the bis-triazole compounds and derivatives thereof as substrates, a series of methods for synthesis of the 1,2,3-bis-triazole derivatives are developed. A variety of novel, highly efficient, simple and easily available ligand catalysts are provided for a click reaction, and the 1,2,3-bis-triazole ligands have obvious effect on accelerating the reaction when used as the ligands and have quite practical application.
Owner:HENAN NORMAL UNIV
Porous membrane based on aminated copolymer microspheres and polyacetal and preparation method of porous membrane
The invention relates to a preparation method for a porous membrane based on aminated copolymer microspheres and polyacetal. The preparation method mainly comprises the steps that 1, styrene-acrylatecopolymer microspheres are prepared to serve as precursor microspheres; 2, diamine is added into a precursor microsphere solution, and surface aminated microspheres are prepared; 3, polymers with opposite charges are alternatively assembled on a substrate to serve as a buffer layer, and then a microsphere layer formed by the surface aminated microspheres and the polyacetal continues to be alternatively assembled; 4, under the action of an external cross-linking agent and a catalyst, the substrate with the buffer layer and the microsphere layer continues to react under the protection of nitrogen, after the reaction is finished, a thin membrane is removed from the substrate, and then the porous membrane can be obtained. According to the preparation method, the uniform large-sized copolymer microspheres synthesized through polymerization of a soap-free emulsion are subjected to surface amination, and then the surface aminated copolymer microspheres and the polyacetal liquid are alternatively mutually assembled to form layers of regular microsphere layer membranes, the microsphere layer membranes are put into a solvent for hypercrosslinking to form the porous membrane, and the method for preparing the regular porous membrane with the controllable thickness is greatly simplified.
Owner:HUBEI UNIV
Imine alkali metal salt and ion liquid as well as application thereof as non-water electrolyte
InactiveCN103626682AEasy to separate and purifyHigh yieldSulfonic acid amide preparationHydroxylamine HydrochlorideIonic liquid
The invention discloses an application of imine alkali metal salt and an ion liquid as non-water electrolyte, and provides an ion liquid consisting of perfluoroalkyl sulfimide alkali metal salt with 'S-perfluoroalkyl sulfimide', perfluoroalkyl sulfimide anion with 'S-perfluoroalkyl sulfimide', as well as sulfonium salt, ammonium salt, microcosmic salt cation. According to the application, an intermediate fluoro-alkyl(S-perfluoroalkyl imino) sulfamide of perfluoroalkyl sulfimide is prepared by reacting (perfluoroalkyl sulfonyl)(perfluoroalkyl sulfinyl) imino with sulfur valence state of +4 and hydroxylamine oxygen sulfonic acid, the routes that fluoro-alkyl(S-perfluoroalkyl imino) sulfamide is prepared from (perfluoroalkyl sulfonyl)(perfluoroalkyl sulfinyl) imino through three steps of chlorination, fluorination and amination are effectively shortened, the operation is simple and convenient, the yield and the purity are high, the alkali metal salt has relatively good thermal stability and hydrolysis resistance, has high conductivity and oxidation potential in the conventional carbonic ester solution, and is good in compatibility with widely applied electrode materials, and the ion liquid can be applied to lithium ion batteries and carbon-based super capacitors.
Owner:HUAZHONG UNIV OF SCI & TECH +1
Preparation method of catalyst for preparing methanol by low-temperature plasma-optical coupling methane and method for preparing methanol
ActiveCN111974393AInhibition of decompositionAvoid reaction conditionsPreparation by oxidation reactionsMetal/metal-oxides/metal-hydroxide catalystsOxidizing agentMixed solution
Owner:NORTHWEST UNIV
Preparation method and application of amino-functionalized mesoporous alumina-based bifunctional adsorbent
InactiveCN103071449BAchieve removalRealize functionOther chemical processesWater contaminantsEngineeringAmino functionalized
Owner:WUHAN UNIV OF TECH
Method for preparing ethyl trans-4-amino-cyclohexanecarboxylate hydrochloride
InactiveCN109280014AImprove efficiencyLow process equipment requirementsCarbamic acid derivatives preparationOrganic compound preparationEthyl acetateReaction step
The invention discloses a method for preparing ethyl trans-4-amino-cyclohexanecarboxylate hydrochloride, and belongs to the field of organic chemistry. Trans-1,4--cyclohexanedicarboxylic acid is usedas an initial material and reacts with anhydrous ethanol to produce intermediate diester A under the condition of a sulfuric acid catalyst, monoester is hydrolyzed by intermediate diester A to obtainintermediate monoacid B, the intermediate monoacid B and DPPA are subjected to Curtius rearrangement to obtain intermediate C, the intermediate C is deprotected by hydrogen chloride ethyl acetate solution to obtain final product ethyl trans-4-amino-cyclohexanecarboxylate hydrochloride I. The process adopted by the invention has the advantages of short reaction steps, cheap raw materials, mild reaction conditions and high yield, and is suitable for industrialized large-scale production.
Owner:CHENGDU BAISHIXING SCI & TECH IND
Method for preparing metal nanomaterial with simulated cell structure
Owner:HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
17alpha-hydroxy-19-norpregn-4,9-diene-3,20-dione preparation process
InactiveCN104774231AAvoid harsh reaction conditionsAvoid reaction conditionsSteroidsGrignard reagentKetone
The present invention provides a 17alpha-hydroxy-19-norpregn-4,9-diene-3,20-dione preparation process, which comprises: adding a reaction substrate 2 to an anhydrous mixing solvent, adding a methyl Grignard reagent, reacting for a certain time at a suitable temperature, carrying out a complete hydrolysis reaction on the obtained intermediate product under an acid condition after the reaction substrate completely reacts, and treating the reaction mixture to obtain the 17alpha-hydroxy-19-norpregn-4,9-diene-3,20-dione, wherein the reaction formula is defined in the instruction. The process of the present invention has advantages of avoidance of harsh reaction condition, high yield up to 88.5%, mild conditions, easy operation, and easy scale-up, and is suitable for industrial production.
Owner:SHANGHAI INST OF PHARMA IND CO LTD +1
Preparation method of 3-substituted phenyl-5-(aminomethyl) oxazolidin-2-one
The invention discloses a preparation method of 3-substituted phenyl-5-(aminomethyl) oxazolidin-2-one. The preparation method comprises the following steps of: enabling substituted aniline to react with (R)-chloro-epoxy propane to get (R)-3-substituted phenylamino-2-hydroxy-chloropropane, further reacting with dibenzyl amine to get (R)-3-substituted phenylamino-1-dibenzyl amino-2-propanol, cyclizing to get (S)-3-substituted phenyl-5-dibenzyl aminomethyl oxazolidin-2-one and finally performing hydrogenation and debenzylation to get (S)-substituted phenyl-5-(aminomethyl) oxazolidin-2-one. A compound obtained by the method disclosed by the invention is of an important intermediate for commercial production of oxazolidinone type antibacterial agents. The method for preparing the 3-substituted phenyl-5-(aminomethyl) oxazolidin-2-one through four-step reaction has the characteristics of few steps, simple operation, low cost and easiness in obtainment of raw materials, mild reaction conditions and the like; and by adopting the method, the production efficiency can be improved, the production energy consumption can be reduced, a safety production coefficient can be further improved, environmental pollution can be reduced, and the preparation method is of an environment-friendly and low-carbon green synthesis method.
Owner:SUZHOU JINGYE MEDICINE & CHEM
Synthetic method of 3-carbonyl-4-aza-5 alpha-androstane-17 beta-carboxylic acid methyl ester
The invention discloses a synthetic method of 3-carbonyl-4-aza-5 alpha-androstane-17 beta-carboxylic acid methyl ester. The method comprises the following steps that 3-carbonyl-4-aza-5-androstene-17 beta-carboxylic acid methyl ester is dissolved in a solvent to react with organic amine formate under catalysis of a metal catalyst; then an object product 3-carbonyl-4-aza-5 alpha-androstane-17 beta-carboxylic acid methyl ester is collected from reaction products. The method of the invention has mild reaction conditions and can realize complete reaction, and the product can have a purity higher than 99% after simple purification. All reagents used in the reaction are easily available. Besides, reaction yield is high; reaction conditions are mild; and the solvent can be recovered for utilization, so as to facilitate industrialized enforcement.
Owner:HUNAN KEREY BIOTECH
Preparation method of 3-substituted phenyl-5-hydroxymethyloxazolidine-2-ketone
ActiveCN102321042AAvoid harsh reaction conditionsIncrease profitOrganic chemistryBulk chemical productionBiochemical engineeringKetone
The invention discloses a preparation method of 3-substituted phenyl-5-hydroxymethyloxazolidine-2-ketone. The preparation method comprises the following steps: carrying out condensation reaction on substituted aniline which is used as a starting material and 3-sustituted-1,2-propanediol so as to synthesize an intermediate (R)-(+)-3-substituted phenylamino-1,2-propanediol; and preparing 3-substituted phenyl-5-hydroxymethyloxazolidine-2-ketone through two-step reaction, wherein the obtained product 3-substituted phenyl-5-hydroxymethyloxazolidine-2-ketone is an important intermediate used for commercially producing oxazolidinone antibacterial agents. The method for preparing 3-substituted phenyl-5-hydroxymethyloxazolidine-2-ketone through two-step reaction has the characteristics of less steps, cheap and available raw materials, mild reaction conditions and the like, and is simple to operate; and by using the method in the invention, production efficiency is improved, production energy consumption is reduced, safe production coefficient is improved, production cost is reduced, environment pollution is reduced, thus the method in the invention is an environmentally-friendly low-carbon green synthesis method.
Owner:SUZHOU JINGYE MEDICINE & CHEM
High basicity composite mahogany sulfonate and its preparation method and use
InactiveCN1990465AHigh Total Base NumberStrong resistance to extreme pressureAdditivesSulfonic acid preparationAlkalinitySulfonate
The invention provides a bimetallic compound sulfonate with high alkalinity, sodium and magnesium containing alkylbenzenesulfonate, the preparing method, and the application of said bimetallic compound sulfonate as lubricant additive. The said sulfonate is characterized by good anti-extreme pressure, anti-oxygen and cleaness, high total alkalinity and adjustable sodium and magnesium content. The method comprises following steps: mixing alkylbenzene sulfonic acid, sodium alkali compound, magnesium alkali compound with low carbon alchol, water, diluting oil and accelerator for reaction; feeding carbon dioxide for carbonation, separating and getting final product. The content of said bimetallic compound sulfonate used as lubricatant additive in oil should be less than 5% by weight.
Owner:CHINA PETROLEUM & CHEM CORP +1
Novel C8-heterocyclic alkylated purine nucleoside analogue and synthetic method thereof
InactiveCN104478883AAvoid harsh reaction conditionsMild reaction conditionsOrganic chemistryChemical recyclingAnti virusBiological activation
The invention discloses a novel C8-heterocyclic alkylated purine nucleoside analogue and a synthetic method thereof and provides a method for synthesizing a C8-heterocyclic alkylated nucleoside analogue by high-efficiency C-H activation. The method adopts raw materials which are easily available, and is moderate in reaction condition and few in reaction steps. The method aims to solve the problems of expensive raw materials, complex process and harsh reaction condition during synthesis of the type of compound, to provide a reference value for synthesis and application of a nucleoside medicine and to provide the raw materials for research of novel anti-virus and antitumor drugs. Meanwhile, the method disclosed by the invention provides an effective method for heterocyclic alkylatation of other nucleosides and analogues of the nucleosides and is wide in industrial application prospect.
Owner:HENAN INST OF SCI & TECH
Preparation method of (E, Z)-2, 4-ethyl decadienoate
InactiveCN109704964AAvoid harsh reaction conditionsHigh degree of continuityOrganic compound preparationCarboxylic acid esters preparationCatalytic effectOxygen
The invention provides a preparation method of (E, Z)-2, 4-ethyl decadienoate. According to the preparation method, n-hexyl aldehyde is taken as an initial raw material, and three step chemical conversion is adopted to prepare a key intermediate 1-bromo heptene; 1-bromo heptene and ethyl acrylate are subjected to coupling reaction under the catalytic effect of a metal catalyst so as to obtain (E,Z)-2, 4-ethyl decadienoate. According to the preparation method, metal catalytic coupling reaction is adopted to replace a step in the prior art that (E, Z)-2, 4-ethyl decadienoate is prepared throughpreparation of an organic copper lithium reagent, water-free oxygen-free harsh conditions are avoided, operation is simplified, reaction efficiency is increased, generation of waste water and waste salt is reduced greatly, equipment investment is reduced, and the preparation method is convenient for industrialization production.
Owner:鼎元(天津)生物医药科技有限公司
Synthesis method of Frutinone compound
InactiveCN110437244AAvoid expensiveSave raw materialsOrganic chemistryPotassium persulfateSynthesis methods
The invention discloses a synthesis method of a Frutinone compound, which comprises the following steps: (1) under the action of Cs2CO3 and a base, substituted ethyl benzoylacetate and substituted 2-chlorobenzoyl chloride react to obtain intermediate 1; (2) the intermediate 1 and boron trihalide are subjected to a hydrolysis reaction to obtain the intermediate 2; (3) the intermediate 2 is oxidizedwith potassium persulfate to obtain a target product. The substituted ethyl benzoylacetate, the substituted 2-chlorobenzoyl chloride, Cs2CO3, boron trihalide and potassium persulfate are used as themain raw materials, and the raw materials are cheap and easy to obtain, thus avoiding the expensive raw materials or precious metal catalysts involved in the existing methods; the synthesis method hasthe advantages of simple operation, mild reaction conditions, environmental friendliness, easy solvent recovery and application, and is suitable for industrial production.
Owner:YANGTZE UNIVERSITY
A kind of linear tin phosphide compound and its preparation method
Owner:UNIV OF JINAN
Preparation method of larotrectinib intermediate
ActiveCN107556226AThe production process is easy to controlPromote the development of economy and technologyOrganic chemistryState of artGrignard reagent
The invention discloses a preparation method of a larotrectinib intermediate (R)-2-(2,5-difluorophenyl)tetrahydropyrrolidine, which comprises the following steps that the larotrectinib intermediate (R)-2-(2,5-difluorophenyl)tetrahydropyrrolidine is prepared by enabling a chiral induction reagent (7aS,12R)-12-phenyl-7a,8,9,10-tetrahydro-12H-naphthol[1,2-e]pyrrolo[2,1-b]oxazine serving as a raw material to react with a Grignard reagent 2,5-difluorophenyl magnesium bromide by means of an addition reaction and a debenzylation reaction. Compared with the prior art, the preparation method has the advantages of simple process, mild conditions, low side reaction, low cost, and adaptability to industrialized production, and can promote the economic and technological development of the bulk pharmaceutical chemical.
Owner:哈尔滨医大药业股份有限公司
Method for preparing lapatinib intermediate
ActiveCN107445879AThe production process is easy to controlPromote the development of economy and technologyOrganic chemistry methodsGrignard reagentBenzotriazole
The invention discloses a method for preparing a lapatinib intermediate (R)-2-(2,5-difluorophenyl)tetrahydropyrrolidine. The method comprises the following steps: by taking taking chiral induced reagent (7aR,10R,12S)-10-(1-benzotriazole)-12-phenyl-7a,8,9,10-tetrahydro-12H-naphthol[1,2-e]pyrrolo[2,1-b][1,3]oxazine and a Grignard reagent 2,5-difluorophenyl magnesium bromide as raw materials, performing a substitution reaction, a reduction reaction and a debenzylation reaction to prepare the lapatinib intermediate (R)-2-(2,5-difluorophenyl)tetrahydropyrrolidine. Compared with the prior art, the method is simple in process, mild in condition, less in side reaction, low in cost and suitable for industrial production and can promote development of the bulk drug economic technology.
Owner:SUZHOU LIXIN PHARMA
The preparation method of 3-substituted phenyl-5-aminomethyl oxazolidin-2-one
The invention discloses a preparation method of 3-substituted phenyl-5-(aminomethyl) oxazolidin-2-one. The preparation method comprises the following steps of: enabling substituted aniline to react with (R)-chloro-epoxy propane to get (R)-3-substituted phenylamino-2-hydroxy-chloropropane, further reacting with dibenzyl amine to get (R)-3-substituted phenylamino-1-dibenzyl amino-2-propanol, cyclizing to get (S)-3-substituted phenyl-5-dibenzyl aminomethyl oxazolidin-2-one and finally performing hydrogenation and debenzylation to get (S)-substituted phenyl-5-(aminomethyl) oxazolidin-2-one. A compound obtained by the method disclosed by the invention is of an important intermediate for commercial production of oxazolidinone type antibacterial agents. The method for preparing the 3-substituted phenyl-5-(aminomethyl) oxazolidin-2-one through four-step reaction has the characteristics of few steps, simple operation, low cost and easiness in obtainment of raw materials, mild reaction conditions and the like; and by adopting the method, the production efficiency can be improved, the production energy consumption can be reduced, a safety production coefficient can be further improved, environmental pollution can be reduced, and the preparation method is of an environment-friendly and low-carbon green synthesis method.
Owner:SUZHOU JINGYE MEDICINE & CHEM
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