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240 results about "Grignard reagent" patented technology

Modified amine curing agent and preparation method thereof, and epoxy resin composite material and preparation method thereof

The invention discloses a modified amine curing agent and a preparation method thereof, and an epoxy resin composite material and a preparation method thereof, and belongs to the field of resin and composite materials. According to the curing agent, a C2-C8 alkyl chain is grafted to a methylene site of 4, 4 '-diaminodiphenylmethane (MDA) through free radical substitution and alkylation reaction, and a molecular structure with a flexible alkyl chain and a rigid benzene ring is formed. The preparation method comprises the following two steps: generating a halogenated intermediate from MDA and a halogen simple substance under certain reaction conditions, alkylating the halogenated intermediate with a Grignard reagent (RMgX), and purifying. The curing agent and epoxy resin are compounded, heated and cured, so that the epoxy resin composite material has relatively high impact strength and fracture toughness, has good tensile strength and hardness, has double functions of reinforcing and toughening, and solves the problem that reinforcing and toughening of traditional epoxy resin are difficult to be compatible; the method is suitable for the fields of aerospace, composite material adhesives and the like with harsh requirements on mechanical properties.
Owner:LUDONG UNIVERSITY

Scalable methods of manufacturing psilocybin

PendingUS20250320240A1Group 5/15 element organic compoundsOrganic grignard reactionsPsilocinPhosphoric Acid Esters
The present disclosure provides methods of manufacturing psilocybin and crystalline psilocybin via a reaction of psilocin and tetrabenzylpyrophosphate in the presence of lithium chloride complex Grignard reagent, which is followed by hydrogenation. Methods of producing psilocin from 4-hydroxyindole or 4-acetoxyindole are also provided.
Owner:COMPASS PATHFINDER LTD

Synthesis method of 7-dehydrocholesterol and derivatives thereof

The invention discloses a synthesis method of 7-dehydrocholesterol and derivatives thereof, which comprises the following steps: cooling a compound (I), cuprous bromide and dimethyl sulfide compound under the protection of inert gas to obtain a reaction system, adding a Grignard reagent (II) or a Grignard reagent (III), stirring, reacting at room temperature, carrying out heating reaction, and cooling to obtain the 7-dehydrocholesterol. Performing post-treatment to obtain a product; if the product is the Grignard reagent (II), the product is 7-dehydrocholesterol and the derivative thereof; if the reagent is the Grignard reagent (III), the product is 25-hydroxy-7-dehydrocholesterol and the derivative thereof. The method is high in total yield, mild in reaction condition, simple in process route, high in product purity, low in three-waste generation amount, simple in post-treatment, environment-friendly and low in equipment requirement, the purity of 95% or above can be obtained through simple recrystallization, and conventional chemical equipment can be used for production.
Owner:DEUTERIUM YIYOU DEUTERIUM (TIANJIN) PHARM CO LTD

Preparation method of post-metallocene catalyst

The invention discloses a preparation method of a post-metallocene catalyst. The method comprises the following steps: by taking quinoline 2-formaldehyde and ortho-aminophenol as raw materials, carrying out reflux reaction on the raw materials and a first solvent to prepare a ligand; dispersing a metal chloride in a second solvent, adding a Grignard reagent, and carrying out a reaction at a low temperature to prepare a methylated metal reagent; and adding a ligand into the methylated metal reagent, reacting at room temperature for 10-12 hours, removing liquid in vacuum, adding part of the second solvent again, stirring, filtering after the product is dissolved, and recrystallizing the filtrate to obtain the product, the metallocene catalyst is obtained by firstly preparing the ligand, then preparing the methylated metal reagent, adding the ligand into the methylated metal reagent for reaction, then stirring by using the second solvent, filtering after the product is dissolved, and recrystallizing the filtrate, so that the operation steps are simple, and the preparation of the ligand does not need water-oxygen treatment operation, and is simple and easy to implement; the preparation cost of the post-metallocene catalyst is reduced, and the method is suitable for industrial large-scale production.
Owner:새틀라이트뉴머티리얼즈알앤디컴퍼니리미티드

Column [n] arene benzoquinone oxime ortho-position functionalized derivative and preparation method thereof

The invention discloses a column [n] arene benzoquinone oxime ortho-position functionalized derivative and a preparation method thereof, and particularly relates to a preparation method for obtaining the column [n] arene benzoquinone oxime ortho-position functionalized derivative by reacting column [n] arene [1] benzoquinone oxime with a Grignard reagent. In the structure of column [n] arene [1] benzoquinone oxime, when alpha, beta-unsaturated ketone and a Grignard reagent are subjected to nucleophilic addition reaction, a 1, 4-addition product with high yield can be obtained, and no 1, 2-addition product exists. The method is mainly characterized in that protons can be removed from hydroxyl of oxime in column [n] arene [1] benzoquinone oxime under an alkaline condition, and oxygen negative ions of the hydroxyl are combined with positively charged metal magnesium atoms in a Grignard reagent to form a six-membered ring transition state, so that R negative ions can attack a No.4 carbon atom of alpha, beta-unsaturated ketone, and a 1, 4-addition reaction is carried out. The preparation method disclosed by the invention is mild in condition and can be carried out without harsh reaction conditions.
Owner:YANAN UNIV

Humidity-heat-resistant bio-based moisture-curing polyurethane hot melt adhesive and preparation method thereof

The invention belongs to the technical field of hot melt adhesives, and relates to a damp-heat-resistant bio-based moisture-curing polyurethane hot melt adhesive, which is prepared from bio-based polyol A, bio-based polyether polyol B, an antioxidant, a flatting agent, isocyanate, a coupling agent and an organic amine catalyst. Wherein the bio-based polyol A is prepared by taking itaconic acid and bio-based diol as raw materials, cooperating with a polymerization inhibitor, synthesizing bio-based polyester diol with the number-average molecular weight of 2500-4000 under the action of a second catalyst, and carrying out addition reaction on double bonds on a side chain of the bio-based polyol A and an n-octyl Grignard reagent under the action of a third catalyst, therefore, the bio-based polyol has a long-chain side group. According to the preparation method, itaconic acid and biological dihydric alcohol are used as raw materials to be matched with an n-octyl Grignard reagent to prepare bio-based polyester polyol with a long-chain side group, the bio-based polyester polyol is applied to the moisture-curing polyurethane hot melt adhesive, and the moisture-curing polyurethane hot melt adhesive with excellent moisture and heat resistance is obtained.
Owner:YANTAI DARBOND TECH

A preparation process of Grignard alcohol

The present invention discloses a preparation process of Grignard alcohol, which uses magnesium and methyl chloride as reaction raw materials, tetrahydrofuran as a solvent, and iodine crystals as an initiator. The Grignard reaction is carried out under nitrogen to generate a Grignard reagent, and then the Grignard reagent reacts with p-chlorobenzophenone by an addition reaction to generate Grignard alcohol. The magnesium includes pre-treated magnesium powder and magnesium strips. By simultaneously using magnesium powder and magnesium strips with specific mass ratios and size ratios and pre-treating them, the present invention can ensure the stable progress of the reaction and improve the reaction yield; in addition, by carrying out the treatment of removing water and peroxides from tetrahydrofuran, while ensuring the process safety, the yield of the Grignard alcohol product can be further improved.
Owner:JIANGXI DONGFU PHARMA CO LTD

Preparation method of SGLT2 inhibitor key intermediate

PendingCN121085890AOrganic chemistrySandmeyer reactionGrignard reagent
The invention discloses a preparation method of an SGLT2 inhibitor key intermediate, and belongs to the technical field of medicinal chemistry. The preparation method comprises the following steps: 1) reacting a compound B with trimethylchlorosilane under an alkaline condition to generate a compound C; 2) reacting the compound C with an aldehyde group reagent on an aromatic ring to generate a compound D; 3) reacting the compound E with a bromination reagent to generate a compound F; 4) preparing the compound F into a Grignard reagent to generate a compound G; 5) carrying out addition reaction on the compound D and a compound G to generate a compound H; and 6) carrying out dehydroxylation and trimethylsilyl protection on the compound H to generate a compound A. According to the preparation method, the risk caused by amplification of the Sandmeyer reaction in the original route is avoided, and meanwhile, the preparation cost of the key intermediate is greatly reduced.
Owner:JIANGSU LIANHUAN PHARMA

Preparation method of (S)-flurbiprofen

The invention relates to the technical field of preparation of small molecule compound medicines, in particular to a preparation method of (S)-flurbiprofen. The method comprises the following steps: dropwise adding a tetrahydrofuran solution of 4-bromo-2-fluorobiphenyl into a mixture of tetrahydrofuran and magnesium, and reacting to generate a Grignard reagent; mixing tetrahydrofuran, (S)-vinyl chloride oxide and ferric acetylacetonate, dropwise adding the Grignard reagent, performing acidolysis ring opening, and performing methylation with methyl iodide and magnesium iodide to obtain an alpha-hydroxyl aromatic carboxylic acid derivative; and reacting with sodium chlorite, nitroxide free radicals and acetonitrile, and oxidizing to obtain the (S)-flurbiprofen. By introducing a chiral induction unit, effective transmission of chiral information is realized in a coupling stage, an original chiral center is not destroyed in a subsequent reaction, and a product is ensured to have a highly consistent configuration. According to the scheme, the technical problem that a method capable of remarkably improving the optical purity and yield of (S)-flurbiprofen is lacked in the prior art can be solved, and the method has good environmental friendliness and industrial application prospects.
Owner:SICHUAN DINGKE PHARMACEUTICAL CO LTD

A kind of preparation method of 3-phenanthrenol

The invention discloses a method for preparing 3-phenanthrenol. The method comprises coupling a compound 3-tert-butoxyphenylboronic acid and o-bromobenzaldehyde to obtain 3'-tert-butoxy-[1,1'-biphenyl]-2-formaldehyde, then reacting 2-(chloromethoxy)-2-methylpropane with magnesium chips in tetrahydrofuran to generate a Grignard reagent, followed by substitution with 3'-tert-butoxy-[1,1'-biphenyl]-2-formaldehyde, and reflux and water separation with p-toluenesulfonic acid to obtain 3'-tert-butoxy-2-(2"-tert-butoxyvinyl)-1,1'-biphenyl, and finally ring closure with methanesulfonic acid and de-tert-butylation to obtain 3-phenanthrenol. The method introduces tert-butyl protection, thereby increasing steric hindrance and reducing isomers during ring closure, and facilitating deprotection conditions. The obtained product can have a purity of more than 99.0% without the need for column chromatography.
Owner:ZHEJIANG CHEMPACIFIC CORP

Synthesis of ferrocene phosphine ligand

PendingCN120230156AOrganic chemistry methodsMetallocenesGrignard reagenttert-Butyllithium
The invention discloses a novel method for synthesizing a ferrocenyl phosphine ligand compound, which comprises the following steps of: reacting a ferrocene compound serving as a starting material with a Grignard reagent and phosphorus trichloride under the action of tert-butyl lithium to generate a ferrocene phosphine ligand, and synthesizing a ferrocene diphosphine ligand in one step. The method is stable and high in practicability, and a novel method for synthesizing the ferrocene ligand compound is provided.
Owner:SHAANXI JUNJING MED BIOMEDICAL TECH CO LTD

Synthesis method of anti-aids drug amdoxovir

This invention provides a method for synthesizing the anti-AIDS drug enovirine. This invention belongs to the field of pharmaceutical preparation technology. The synthesis method includes the following steps: (1) SM1 compound reacts with Grignard reagent and then reacts with SM2 compound to obtain compound III; (2) Compound III undergoes oxidation reaction to obtain compound II; (3) Compound II undergoes demethylation reaction under the action of demethylation reagent to obtain compound I; (4) Compound I undergoes ethylation reaction to obtain enovirine. The synthesis route of this invention effectively avoids the use of highly toxic cyanide reagents and expensive heavy metal catalysts. At the same time, the reaction conditions of this route are simple and mild, with high yield, and have excellent industrialization prospects.
Owner:成都艾迪医药技术有限公司 +2

Preparation method of rosemeltirol

The invention discloses a preparation method of rosmeltirol, and belongs to the technical field of chemical synthesis. The method comprises the following steps: taking a compound I as an initial raw material, generating a compound II through base catalysis, and performing bromination reaction to obtain a compound III; carrying out Suzuki coupling reaction on the compound III and isopropenyl boronic acid pinacol ester to obtain a compound IV; then reacting with 2, 6-dichloro-4-aminophenol to generate a key intermediate V; performing diazotization coupling reaction to obtain a compound VI, and performing ring closing reaction to form a compound VII; and finally, carrying out hydrogenation reduction to obtain the target product rosimeltirol. The conventional catalyst is adopted to replace a noble metal system, industrial easily-available raw materials are selected to avoid the use of a Grignard reagent, the yield of each step is up to 85% through optimization of reaction conditions, and the purity of a final product reaches 99.8% or above; meanwhile, the raw material cost is reduced, the emission of three wastes is reduced, the operation safety is improved, and a reliable technical scheme is provided for large-scale production of the rosmeltirol.
Owner:NANTONG CHANGYOO PHARMATECH CO LTD

Chiral hydrosilane compound as well as preparation method and application thereof

The invention discloses a chiral hydrosilane compound as well as a preparation method and application thereof. The structural formula of the chiral hydrosilane compound is shown as a formula (I). The chiral hydrosilane compound can be prepared by two methods, one method comprises the following steps: synthesizing tert-butyldihydrosilane from cheap and easily available phenyl silane through a Grignard reagent reaction, adding a ligand and hexamethyldisilylamino potassium to react with benzyl alcohol in a copper tetracyano hexafluorophosphonate catalysis manner, and carrying out reduced pressure distillation to obtain the chiral hydrosilane compound. And finally, synthesizing a hydrogen silane compound with chirality. And the other method comprises the step of adding a brominated compound and cesium carbonate in a copper metal catalysis process to generate the chiral hydrosilane compound. According to the invention, the range of the product is widened to a great extent, and a foundation is laid for subsequent application and transformation. # imgabs0 #
Owner:HANGZHOU NORMAL UNIVERSITY

Grignard reagent continuous synthesis device and system

The utility model relates to a Grignard reagent continuous synthesis device and system, the device comprises a tubular reactor main body and a stirrer, the lower end and the upper end of the reactor main body are respectively provided with a liquid feed port and a discharge port, and the top of the reactor main body is provided with a magnesium powder feeding unit for connection; a jacket for heating and cooling reaction materials is arranged outside the reactor main body; the stirrer comprises a motor and a supporting rod connected with the output end of the motor, the motor is arranged at the top of the reactor main body, the supporting rod extends downwards from the top in the reactor main body, a mixing assembly is arranged on the supporting rod and comprises a push type stirring rod, and holes are distributed in the push type stirring rod. According to the utility model, continuous and efficient mixing of raw materials and magnesium metal and rapid heat transfer and temperature control can be realized, so that the reaction time is greatly shortened; and the flowing process of the materials in the reaction main body is close to a plug flow process, so that the backmixing of the materials is reduced, the radial mixing of the materials is increased, and the product quality of the Grignard reagent is improved.
Owner:SHANGHAI MAIKAITAI FLUID TECHNOLOGY CO LTD +1

Synthesis method of triphenylphosphine

The invention relates to a synthesis method of triphenylphosphine, which belongs to the technical field of organic synthesis, and comprises the following steps: Step 1: adding a solvent, magnesium chips and an initiator into a reaction bottle, and heating to 50-60 DEG C; 2, dropwise adding a mixed solution of benzene halide and phosphorus trichloride, and after addition is completed, carrying out a heat preservation reaction; 3, after the reaction is finished, the temperature is reduced to the room temperature, water is added for washing and layering, an organic phase is concentrated, the solvent is recycled, and triphenylphosphine is obtained. According to the method, benzene halide and phosphorus trichloride are used as raw materials and react with magnesium chips through a one-pot method in a solvent to directly synthesize triphenylphosphine, compared with a traditional synthesis method, a Grignard reagent does not need to be prepared step by step, high energy consumption caused by low-temperature reaction conditions during subsequent Grignard reagent addition is not needed, the process is safer and more efficient, energy consumption can be effectively reduced, and the method is suitable for industrial production. Compared with a traditional synthesis method, the method has the advantages of no high risk of a sodium method process, safety and environmental protection pressure relief, simple overall process, high yield and suitability for industrial large-scale production.
Owner:LIAONING ZETAI BIOTECHNOLOGY CO LTD

Process for the preparation of the drug centhaquine for the treatment of hemorrhagic shock

This invention provides a method for preparing Centhaquine, a drug for treating hemorrhagic shock. Specifically, the preparation method provided by this invention includes the following steps: (S1) providing compound II and compound IV; wherein compound II is prepared by the following method, which includes the steps of: (A) reacting compound I with 1,2-dibromoethane in a first solvent in the presence of base 1 to obtain compound II; and compound IV is prepared by the following method, which includes the steps of: (B) reacting compound III with pinacol diborate in a second solvent in the presence of Grignard reagent to obtain compound IV; (S2) preparation of compound A; and reacting compound II and compound IV in a third solvent in the presence of a catalyst and base 2 to obtain Centhaquine. The preparation method of this invention has a simple and safe synthetic route and operation, readily available raw materials, simple post-processing, high yield, and is suitable for industrial production.
Owner:SHANGHAI TIANCI BIOLOGICAL VALLEY BIOLOGICAL ENG

Lithium metal negative electrode and preparation method and application thereof

The invention discloses a lithium metal negative electrode and a preparation method and application thereof.A Grignard reagent with the molecular formula being RMgX is dissolved in an organic solvent to form a uniform solution, X in the molecular formula RMgX represents chlorine or bromine, R represents an organic substituent and comprises one of methyl, ethyl, propyl, n-butyl or phenyl, the solution reacts with lithium metal in a spin coating or spraying mode, and the lithium metal negative electrode is obtained. And the lithium metal negative electrode with the oxide layer removed and the surface protected by the lithium-magnesium alloy coating is obtained through cleaning with an organic solvent, and the preparation method is simple and efficient. The obtained lithium-magnesium alloy protective layer can effectively prevent direct contact between a lithium negative electrode and electrolyte, and side reaction in the charging and discharging process is inhibited. Besides, compared with a pure lithium negative electrode, the lithium-magnesium alloy protective layer with the double-layer structure has higher strength and can inhibit SEI fracture caused by volume expansion of the lithium negative electrode in the charging and discharging process, so that generation of dendritic crystals and loss of electrolyte are inhibited, the reversibility of lithium deposition is improved, and the cycle life of the battery is further remarkably prolonged.
Owner:CHANGCHUN INSTITUTE OF APPLIED CHEMISTRY CHINESE ACADEMY OF SCIENCES

Alpha-aminophosphoryl derivative as well as preparation method and application thereof

The invention discloses an alpha-aminophosphoryl derivative as well as a preparation method and application thereof. The method comprises the following steps: by taking a quinoline derivative as a raw material and tetrahydrofuran (THF) as a solvent, adding boron trifluoride diethyl etherate in a nitrogen system at the reaction temperature of 0 DEG C, stirring for 15 minutes, reducing the temperature of the reaction system to T1 (-60 DEG C to-30 DEG C), adding a Grignard reagent into the reaction system, and reacting for 30 minutes to obtain a solution A; dissolving a phosphorus reagent in the organic solvent at room temperature in a nitrogen atmosphere to obtain a solution B; and adding the solution A into the solution B, reacting for 6-15 hours at the reaction temperature T2 (0-50 DEG C), and after the reaction is finished, extracting, concentrating and carrying out column chromatography to obtain the target product alpha-aminophosphoryl derivative. The invention provides a novel synthetic route for preparing the alpha-aminophosphonyl derivative, and various phosphorus reagents such as diaryl phosphorus oxide and phosphite ester can be compatible with the reaction. The alpha-aminophosphoryl derivative synthesized by the invention has a good antibacterial effect on gram-positive bacteria, especially staphylococcus aureus.
Owner:YANTAI UNIV +1

Preparation method of cresol trozole trisiloxane intermediate

The invention discloses a preparation method of a cresol trozole trisiloxane intermediate, and belongs to the technical field of fine chemical engineering. The preparation method comprises the following steps: by taking 2, 6-dibromo-4-methylphenol as a raw material, reacting with 3, 4-dihydropyran under the action of p-toluenesulfonic acid, so as to generate an intermediate 2-(2, 6-dibromo-4-methylphenoxy) pyran; reacting with sodium methoxide under the action of a catalyst to generate an intermediate 2-(2-bromo-4-methyl-6-methoxyphenoxy) pyran; then generating a Grignard reagent, carrying out coupling reaction on the Grignard reagent and 3-bromine-2-methallyl, finally reacting with benzotriazole lithium salt, and carrying out acidolysis deprotection to obtain the cresol trozole trisiloxane intermediate. The raw materials are available in the market, the overall yield is high, and a route reference is provided for synthesis of the compounds.
Owner:安徽英特美科技有限公司

Highly efficient stable grignard reagent and green preparation method thereof

This invention relates to the field of organic synthesis technology, specifically to a highly efficient and stable Grignard preparation and its green preparation method. By weight, it comprises 8-18 parts of a magnesium source, 40-92 parts of a halogenated hydrocarbon, 150-200 parts of a green solvent, 15-20 parts of ethylene glycol dimethyl ether, and 2.3-3.2 parts of a synergistic stabilizer. The green solvent is 2-methyltetrahydrofuran, or a composite solvent with a weight ratio of 2-methyltetrahydrofuran:methyl tert-butyl ether of 150-160:40-50. The synergistic stabilizer is composed of 1.5-2.0 parts of N,N,N',N'-tetramethylethylenediamine and 0.8-1.2 parts of butylated hydroxytoluene, or composed of 1.5-2.0 parts of N,N,N',N'-tetramethylethylenediamine and 1.0 part of phenothiazine. This invention uses a green solvent system to replace traditional toxic and harmful solvents, and combines it with a solvent recovery process to achieve solvent recycling, which greatly reduces waste emissions and makes the production process safer and more environmentally friendly, in line with the development direction of green chemical industry.
Owner:LANZHOU HONGSHENG FINE CHEM CO LTD

Synthesis method of teprenone

The invention discloses a synthesis method of teprenone, which comprises the following steps: dissolving farnesyl acetone in a solvent, and reacting with a Grignard reagent at low temperature to obtain geranyl linalool; the method comprises the following steps: mixing geranyl linalool, alkyl acetoacetate and an organic aluminum catalyst, reacting under a heating condition, adding a dilute acid solution and an organic extraction solvent into the reacted mixed solution, extracting, separating an organic phase to obtain a teprenone crude product, and carrying out reduced pressure distillation purification to obtain teprenone, the yield and the purity of the teprenone in industrial production are improved.
Owner:SUZHOU HANDE CHUANGHONG BIOCHEMICAL TECH CO LTD

A preparation method of 1-aryl-3-arylsulfinylbicyclo[1.1.1]pentane

The present invention discloses a method for preparing 1-aryl-3-arylsulfinylbicyclo[1.1.1]pentane. Under inert gas protection, an aryl Grignard reagent is reacted with [1.1.1] propeller alkane, and the resulting intermediate solution is reacted with an SO2 source. After the reaction is completed, 1-aryl-3-arylsulfinylbicyclo[1.1.1]pentane is obtained by post-processing. The present invention achieves efficient preparation of 1-aryl-3-arylsulfinylbicyclo[1.1.1]pentane without adding any catalyst, and has low raw material cost, easy operation, mild conditions, and high reaction yield, and has broad application value.
Owner:ZHEJIANG UNIV OF TECH

Preparation method of pyruvic acid-1-13C

The invention provides a preparation method of pyruvic acid-1-13C, and relates to the technical field of chemical drugs, and the preparation method comprises the following steps: carrying out reaction and post-treatment on 13C-carbon dioxide and a Grignard reagent to obtain pyruvic acid-1-13C; wherein the Grignard reagent comprises a Grignard reagent obtained by reacting magnesium with acetyl halide. The technical problems that in the prior art, a pyruvic acid-1-13C synthesis method has safety risks, raw materials are not easy to obtain, the number of reaction reagent types is large, the number of process steps is large, and the yield is low are solved, the technical effects that safety and environmental protection are achieved, the raw materials are easy to obtain, the process is simple, and the synthesis route is short are achieved, and the obtained pyruvic acid-1-13C is high in purity and high in yield. And clinical test requirements can be met.
Owner:BEIJING HUAGEN ANBANG TECH CO LTD +1

Synthesis of aluminum precursors without use of pyrophoric compounds and related compositions and related methods

Methods for forming a vapor deposition precursor are provided. The method comprises contacting an aluminum halide compound, an alkoxy aluminum compound, and a Grignard reagent to form the vapor deposition precursor. The vapor deposition precursor comprises an dialkyl aluminum alkoxide compound. The vapor deposition precursor is formed without use of a pyrophoric compound. Related compositions, related precursors, and related methods are also provided, among other things.
Owner:ENTEGRIS INC

Synthesis method of polysubstituted cyclopropyl carbonyl compound

The invention discloses a synthesis method of a polysubstituted cyclopropyl carbonyl derivative, and belongs to the technical field of organic synthesis and the technical field of medicine synthesis. The method comprises the following steps: (1) taking substituted olefin as a raw material, and obtaining alpha-chlorocyclobutanone through [2 + 2] cycloaddition and reduction reaction; and (2) carrying out rearrangement reaction on the alpha-chlorocyclobutanone and different types of Grignard reagents or organic lithium reagents to obtain the polysubstituted cyclopropyl carbonyl derivative. The synthesis method provided by the invention has the advantages of wide substrate range, good functional group compatibility, mild reaction conditions, no need of preparation of active intermediates or use of expensive transition metal catalysts, simple operation, capability of obtaining various types of cyclopropyl carbonyl compounds, and the like. The practicability of the method is further shown through later-stage functional group modification of complex bioactive molecules and abundant derivatization of polysubstituted cyclopropyl carbonyl products of the complex bioactive molecules.
Owner:KUNMING INST OF BOTANY CHINESE ACAD OF SCI

A kind of C 2 Symmetric chiral bisphosphine ligand and its application in asymmetric hydrogenation reaction

The present invention discloses a C2-symmetric chiral bisphosphine ligand and its application in asymmetric hydrogenation reactions. The synthesis of this new type of chiral bisphosphine ligand can be prepared starting from the chiral raw material Ugi's amine, through deprotonation, followed by a tandem reaction with phosphine chloride and Grignard reagent. The synthesis method is simple, with variable structures and easy to control. At the same time, the present invention discloses a catalyst formed by this new type of chiral bisphosphine ligand and metal, which exhibits excellent catalytic activity and stereoselectivity in asymmetric hydrogenation and can be applied to the preparation of chiral drugs such as ibuprofen, naproxen, and alfloprofen.
Owner:SHENZHEN CATALYS SCI & TECH CO LTD

[BMIM] Cl (at) MCM-41 catalyst and method for synthesizing methyl trichlorosilane by using [BMIM] Cl (at) MCM-41 catalyst

The invention relates to a [BMIM] Cl (at) MCM-41 catalyst and a method for synthesizing methyl trichlorosilane, the preparation method of the catalyst comprises the following steps: a) preparing an MCM-41 mesoporous molecular sieve by adopting a hydrothermal synthesis method, the specific method for preparing the MCM-41 mesoporous molecular sieve is as follows: taking cetyltrimethylammonium bromide (CTAB) as a template agent, taking tetraethyl orthosilicate (TEOS) as a silicon source, and adopting a hydrothermal synthesis method for preparing the MCM-41 mesoporous molecular sieve; the preparation method comprises the following steps of: mixing and stirring the MCM-41 molecular sieve serving as a raw material and tetramethylammonium hydroxide (TMAOH) serving as an alkali solution to form gel, dealcoholizing, crystallizing, washing, drying and calcining to obtain the MCM-41 mesoporous molecular sieve. The [BMIM] Cl (at) MCM-41 is used as the catalyst for synthesizing methyl trichlorosilane by a Grignard reagent method, the mesoporous structure of the MCM-41 improves the diffusion efficiency of reactants, and the structure is matched with the molecular size of the ionic liquid to form a uniformly dispersed active center and shorten the contact path of the reactants.
Owner:ZHEJIANG RUIHENG ELECTRONIC MATERIALS CO LTD

Continuous reaction equipment for preparing sartan biphenyl

The utility model provides continuous reaction equipment for preparing sartan biphenyl and belongs to the technical field of reaction equipment. Comprising a support frame; the Grignard reaction cabin is stably mounted on the supporting frame and is used for carrying out a preparation reaction of a Grignard reagent; the coupling reaction cabin is stably mounted on the support frame and is used for carrying out coupling reaction to generate the sartan biphenyl; and the cooling part is stably mounted on the supporting frame. Through cooperation of the Grignard reaction cabin, the coupling reaction cabin and the cooling part, the temperature requirement of the coupling reaction is met under the condition of not additionally arranging heating equipment, the energy consumption and the cost are reduced, and meanwhile through structural cooperation of a pressure relief opening formed in one side of the gas storage cabin, an internal sealing plug, a spring and a plurality of gas inlet channels, the pressure relief opening is formed in the other side of the gas storage cabin. And the pressure can be automatically relieved when the air pressure in the air storage bin is too high.
Owner:XINXIANG CITY SANXIN SCI & TECH CO LTD

A green synthetic process of alkynol double grignard reagent

The method discloses a green synthesis process of acetylene alcohol double Grignard reagent, and the synthesis process comprises the following steps: dissolving benzyl chloride in an organic solvent to prepare solution A, adding metal magnesium to solution A to initiate a reaction, and preparing an initiation reaction solution; (2) dissolving benzyl chloride and acetylene alcohol substances in an organic solvent to prepare solution B; (2) adding solution B in step (2) to the initiation reaction solution in step (1) dropwise to perform a reaction, and preparing acetylene alcohol double Grignard reagent. The application provides a new synthesis method for synthesizing acetylene alcohol double Grignard reagent by using benzyl magnesium chloride, which can avoid a coupling side reaction between benzyl Grignard reagent and benzyl chloride, and does not need excessive metal magnesium.
Owner:SHANGYU NHU BIOCHEM IND