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328 results about "Grignard reagent" patented technology

Synthesis method of dialkyl amino alcohol

The invention discloses a synthesis method of dialkyl amino alcohol. The dialkyl amino alcohol is obtained by reacting dialkyl amino ester with a Grignard reagent. According to the synthetic route provided by the invention, the overall synthesis condition is mild, the used raw materials are easy to obtain, and the toxicity is relatively low.
Owner:FUJIAN CHUNMING NEW MATERIAL TECH CO LTD

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

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 6-methyl-5-octylene-2-ketone

The invention discloses a preparation method of 6-methyl-5-octylene-2-ketone, and belongs to the technical field of organic synthesis. According to the method, 5-chloro-2-pentanone is taken as a starting raw material, carbonyl protection is carried out with trimethyl orthoformate under the catalysis of acid, then a Grignard reagent is prepared, condensation dehydration is carried out on the Grignard reagent and 2-butanone, deprotection is carried out under the acidic condition, and 6-methyl-5-octylene-2-ketone is prepared with high yield, the raw materials are easy to obtain and low in price, and the reaction can be catalyzed by using a conventional catalyst.
Owner:JINAN ENLIGHTEN BIOTECH CO LTD

Method for producing hexafluorobutadiene, continuous production system and application thereof

The invention relates to the technical field of organic chemical synthesis, and particularly discloses a method for producing hexafluorobutadiene, a continuous production system and application thereof. The method for producing hexafluorobutadiene comprises the following steps: (1) bromination reaction: reacting tetrafluoroethylene with liquid bromine to generate dibromotetrafluoroethane; (2) telomerization reaction: reacting the dibromo tetrafluoroethane with tetrafluoroethylene under the action of a catalyst to generate dibromo octafluorobutane; the catalyst is cuprous bromide; and (3) elimination reaction: reacting the dibromo octafluorobutane under the action of a Grignard reagent to generate hexafluorobutadiene. The method provided by the invention has the advantages of simple process, easily available raw materials, high production efficiency, continuous production, low production cost and industrial mass production value.
Owner:ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD

Preparation method of metal organic complex

The invention relates to the technical field of synthesis of metal organic complexes, in particular to a preparation method of a metal organic complex, and aims to solve the problems that the metal organic complex is tedious to prepare, low in yield, high in cost, incapable of meeting industrial production requirements and the like in the prior art. The preparation method of the metal organic complex comprises the following steps: carrying out Grignard reaction on a Grignard reagent and (dimethylamino) acetone to prepare a first product; wherein the Grignard reagent comprises R-MgX, R is selected from any one of C1-C2 alkyl groups, and X is selected from any one of chlorine, bromine and iodine; the general formula of the first product is as shown in the following formula (I): # imgabs0 # (I); carrying out a complexation reaction on the first product and a salt of a first metal M to prepare a metal organic complex; the general formula of the metal organic complex is as shown in the following formula (II): # imgabs1 # (II); m is selected from any one of copper and nickel.
Owner:JIANGSU SINOCOMPOUND CATALYST

Method for preparing pyridazinone compound and application of pyridazinone compound

The invention belongs to the technical field of pharmacy, and particularly relates to a method for preparing a pyridazinone compound and application of the pyridazinone compound, and the method comprises the following steps: step 1, reacting a compound as shown in a formula V with a Grignard reagent to obtain a compound as shown in a formula IV; 2, reacting the compound shown in the formula IV with succinic anhydride to obtain a compound shown in a formula III; 3, reacting the compound shown in the formula III with hydrazine hydrate to obtain a compound shown in a formula II; 4, oxidizing the compound shown in the formula II to obtain a pyridazinone compound; the pyridazinone compound or the pharmaceutically acceptable salt or prodrug of the pyridazinone compound can be used for inhibiting the activity of MET protein kinase and the mutant form of the MET protein kinase, and especially can be used as a Tepotinib intermediate.
Owner:SHENZHEN HUAXIAN PHARMA TECH CO LTD

Low-density high-thermal-conductivity composite silicone oil cooling liquid and preparation method thereof

The invention relates to the field of immersed coolants, and discloses a low-density high-thermal-conductivity composite silicone oil coolant and a preparation method thereof, the method comprises preparation of naphthyl-terminated aryl silicone oil and application of the naphthyl-terminated aryl silicone oil to a base liquid of the silicone oil coolant, and the thermal conductivity of the silicone oil coolant is improved. Dissolving dimethyldichlorosilane in tetrahydrofuran, dropwise adding a naphthalene Grignard reagent into the mixed solution, and after the reaction is finished, carrying out quenching, extraction and other processes to obtain dimethylnaphthalene aryl chlorosilane; adding a potassium carbonate solution into the dimethyl naphthyl aryl chlorosilane, and extracting after reaction to obtain dimethyl-naphthyl siloxane alcohol; adding a tin catalyst into the dimethyl-naphthyl siloxane alcohol, carrying out vacuum reaction, rectifying and purifying to obtain tetramethyl dinaphthyl disiloxane; the naphthyl-terminated aryl silicone oil is prepared by taking DMC as a raw material, KOH potassium as a catalyst and tetramethyl dinaphthyl disiloxane as an end capping agent. The composite silicone oil cooling liquid with low density, high specific heat capacity and stable structure is prepared by stirring, mixing and compounding.
Owner:HUBEI XINGRUI SILICON MATERIAL CO LTD

Preparation method of perfluorohexyl octane

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of perfluorohexyl octane. The preparation method comprises the following steps: by taking perfluorohexyl ethyl iodide as a raw material, firstly carrying out Grignard reagent exchange with a reagent A, and then carrying out nucleophilic addition reaction with n-hexanal to obtain a compound III; carrying out esterification and substitution on the compound III to prepare a compound V, or carrying out an Apple substitution reaction to prepare the compound V; and carrying out reduction reaction on the compound V, rectifying and purifying to obtain a target product. The reagent A comprises an isopropyl magnesium chloride tetrahydrofuran solution, a methyl magnesium chloride tetrahydrofuran solution, a methyl magnesium bromide tetrahydrofuran solution, an ethyl magnesium chloride tetrahydrofuran solution, an ethyl magnesium bromide tetrahydrofuran solution and / or a phenyl magnesium bromide tetrahydrofuran solution. According to the method, the perfluorohexyl ethyl iodide and the n-hexanal are used as raw materials to prepare the perfluorohexyl octane, isomer impurities are fundamentally avoided, and the method has the advantages that purification is easy, the yield is high, the product purity is high, and industrial production is facilitated.
Owner:CHONGQING HUABANGSHENGKAI PHARM CO LTD

Long-acting environment-friendly flame-retardant anti-static rubber pad and preparation method thereof

The invention discloses a long-acting environment-friendly flame-retardant anti-static rubber pad and a preparation method thereof, and relates to the technical field of rubber pads. The long-acting environment-friendly flame-retardant anti-static rubber pad prepared by the application comprises the static conductive layer at the bottom layer and the static dissipation layer attached to one surface of the static conductive layer. The static dissipation layer comprises modified nitrile rubber, acrylate resin and a first auxiliary agent; and the static conductive layer comprises modified nitrile rubber, butadiene styrene rubber, polyurethane resin and a second auxiliary agent. Wherein the modified nitrile rubber is obtained by reacting a Grignard reagent RMgBr with cyano groups in nitrile rubber, converting the cyano groups into carbonyl groups, and introducing a phosphorus-containing organic compound into the nitrile rubber by utilizing aldol condensation. The rubber pad prepared from the modified nitrile rubber is excellent in anti-static performance, has flame retardance, is long-acting and environment-friendly, and has a wide application prospect.
Owner:CHUANGXUANBAO PANTUO ANTI STATIC TECH SHANGHAI CO LTD

Magnesium battery electrolyte and application thereof

The invention belongs to the technical field of electrolyte, and discloses magnesium battery electrolyte added with indium chloride and application of the magnesium battery electrolyte, the magnesium battery electrolyte is composed of one or more of a Grignard reagent system, an MACC system, an Mg-TFSI system, an Mg-B system and Mg-HMDS and indium chloride, the indium chloride is an additive which can be dissolved in the magnesium electrolyte without the assistance of a large amount of aluminum trichloride, and through the synergistic effect of electrolyte components and the indium chloride, the cycle life of the magnesium battery is prolonged, and the specific discharge capacity of the magnesium battery is improved.
Owner:CHANGZHOU UNIV

Preparation method of sacubitril intermediate

The invention discloses a preparation method of a sacubitril intermediate, which comprises the following steps: taking N-tert-butoxycarbonyl-L-serine ester as an initial raw material, reacting with sulfonyl chloride under the catalysis of an alkaline substance to obtain N-(tert-butoxycarbonyl)-O-sulfonyl-L-serine ester, activating hydroxyl in the compound by sulfonate, and reacting with sodium hydroxide to obtain the sacubitril intermediate. The preparation method comprises the following steps: reacting (R)-3-([1, 1 '-biphenyl]-4-yl)-2-(tert-butoxycarbonyl) amino) propionate with a Grignard reagent under the catalysis of copper to generate (R)-3-([1, 1'-biphenyl]-4-yl)-2-(tert-butoxycarbonyl) amino) propionate, and finally reducing ester groups into hydroxyl groups under the action of a catalyst and a reducing agent to generate (R)-tert-butyl (1-([1, 1 '-biphenyl]-4-yl)-3-hydroxypropane-2-yl) carbamate. The preparation method has the advantages of simple preparation process route, cheap and easily available raw materials, short synthesis route, mild reaction conditions, simplicity and convenience in operation and high yield, and has better application value and economic benefit.
Owner:ZHEJIANG UNIV OF TECH

Risk control method and system for Grignard reagent production process

The invention discloses a risk control method and system for a Grignard reagent production process, and relates to the technical field of chemical safety and engineering. Comprising the following steps: obtaining Grignard reagent synthesis reaction heat balance data and Grignard reagent synthesis system material potential decomposition risk information through reaction safety risk analysis; determining a dangerous scene of the Grignard reagent production process; and establishing a Grignard reagent risk control model based on the heat balance data, the material potential decomposition risk information and the dangerous scene, obtaining risk control parameters, and realizing risk control of the Grignard reagent production process. Thermodynamic quantitative data in the Grignard reagent synthesis reaction process is obtained through testing, a potential risk scene in the Grignard reagent production stage is further determined through scene analysis, risk control measures are established according to dangerous scene characteristics, and the safety problem of the Grignard reagent production process is solved.
Owner:SHENYANG RES INST OF CHEM IND

A reaction device for Grignard reaction

The utility model relates to a reaction device for Grignard reaction, which comprises: a Grignard reagent batching kettle; a Grignard reactor, wherein the Grignard reactor comprises a reactor body, a second jacket formed on the outer wall of the reactor body, a second agitator rotatably mounted in the reactor body and extending to the outside thereof, a second motor mounted on the top of the reactor body and connected to the second agitator, a plurality of second feed ports opened on the top of the reactor body, and a second discharge valve mounted on the bottom of the reactor body; a feed delivery component, wherein the feed delivery component comprises a feed delivery pipe connecting the first discharge valve and any of the second feed ports, a first flow meter mounted on the feed delivery pipe, and a first regulating valve mounted on the feed delivery pipe and located downstream of the first flow meter. In this way, the problems of overheating (i.e., energy accumulation) and spraying that may exist when a single reactor is used can be avoided.
Owner:浙江华佐天翼化工科技有限公司 +1

Preparation method and device of prothioconazole

The invention provides a preparation method and device of prothioconazole. The preparation method comprises the following steps: carrying out Grignard reaction on o-chlorobenzyl chloride and magnesium powder in a mixed solvent of toluene and 2-methyltetrahydrofuran; the method comprises the following steps: carrying out Grignard addition reaction on a Grignard reagent and 2-chloro-1-(1-chlorocyclopropyl) ethanone; the preparation method comprises the following steps: carrying out substitution reaction on 1-chloro-2-(1-chlorocyclopropyl)-3-(2-chlorphenyl) propanol and hydrazine hydrate in an alcohol solvent; the preparation method comprises the following steps: carrying out ring closing reaction on 2-(1-chlorocyclopropyl)-1-(2-chlorphenyl)-3-hydrazino-2-alcohol, a formaldehyde solution, a sodium thiocyanate solution and a sodium hydrogen sulfate solution; the preparation method comprises the following steps: carrying out oxidation reaction on 2-(2-chlorocyclopropyl)-3-(2-chlorphenyl)-2-hydroxypropyl)-1, 2, 4-triazolidine-3-thioketone, air and inorganic alkali, so as to obtain prothioconazole. The method can improve the efficiency of the oxidation reaction and the yield and purity of prothioconazole, and is more suitable for industrial production of prothioconazole.
Owner:TIANJIN ASYMCHEM MEDICAL SCI & TECH DEV 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

Insecticidal double water agent and preparation method thereof

InactiveCN119684184ABiocideOrganic chemistryGrignard reagentThiosulfonic Acids
The invention provides an insecticidal double-water agent and a preparation method thereof, and relates to the technical field of pesticides, the insecticidal double-water agent comprises the following raw materials by weight: 90-95 parts of a sulfonation liquid, 3-8 parts of 4-chlorobenzyl chloride and 4-9 parts of magnesium chips. The preparation method specifically comprises the following steps: S1, preparing a Grignard reagent; s2, preparing concentrated sulfonation liquid; s3, reacting dimehypo with chlorine to prepare chloride; s4, enabling the Grignard reagent to react with chloride to generate 2-dimethylamino-2-p-chlorobenzyl chloro-1, 3-sodium dithiosulfonate propane; s5, enabling the 2-dimethylamino-2-p-chlorobenzyl chloro-1, 3-sodium dithiosulfonate propane to react with sodium thiosulfate, so as to prepare a sodium p-methanesulfonate insecticidal double-water agent; and S6, performing post-treatment on the sodium methanesulfonate insecticidal double water agent, and adding a synergist to obtain a final product. The dimehypo reagent prepared by the method disclosed by the invention is not crystallized at the high concentration of 36-43%, and the content of sodium hyposulfite is lower than 0.1%.
Owner:GNSG ANHUI HONG SIFANG

Preparation method of substituted benzoate derivative

The invention provides a preparation method of a substituted benzoate derivative, which comprises the following steps: reacting zinc powder with a compound A in an organic solvent under the protection of inert gas to obtain a compound B containing a zinc reagent, coupling the compound B with a compound C under the action of a nickel catalyst and a metal Grignard reagent to generate a compound D, and separating the compound D from the compound C to obtain the substituted benzoate derivative. The method for preparing the final product is simple and efficient, the cost is reduced, and production is facilitated.
Owner:SHANGHAI HAOYUAN CHEMEXPRESS CO LTD

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

Preparation method of 2-(4-bromophenyl) norcamphane

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of 2-(4-bromophenyl) norcamphane. According to the invention, the proper catalyst is selected to promote the norbornene to be directly added with the bromobenzene Grignard reagent, so that the use of expensive raw materials is avoided, the reaction difficulty is reduced, and the reaction can be smoothly carried out, thereby effectively improving the reaction yield of the 2-phenyl norcamphane. According to the bromination reaction of the 2-phenyl norcamphane, proper catalysts and reaction conditions are selected, and the selectivity of para-products is improved, so that the product yield of the 2-(4-bromophenyl) norcamphane is improved.
Owner:HEBEI FANKE NEW MATERIALS 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

4, 7-diaryl thieno [2, 3-d] pyridazine iridium complex as well as preparation method and application thereof

The invention relates to the technical field of luminescent materials, in particular to a 4, 7-diaryl thieno [2, 3-d] pyridazine iridium complex as well as a preparation method and application thereof, and structurally designs and synthesizes a 4, 7-diaryl thieno [2, 3-d] pyridazine ligand taking thieno pyridazine as a basic framework. In the synthesis process, an S atom on a thiophene ring of the thiophene double Weinreb amide has electron deficiency, so that a Grignard reagent is only positioned and substituted on one side (the electron-deficient side) with the S atom, and further the positioned and substituted 4, 7-diaryl thieno [2, 3-d] pyridazine ligand and the cyclometalated iridium complex thereof are generated. The benzothienopyridazine ligand disclosed by the invention shows a strong conjugation effect, and after the cyclometalated iridium complex of the benzothienopyridazine ligand is prepared into an organic electroluminescent device, the device shows excellent red light emission.
Owner:HUBEI UNIV OF ARTS & SCI