24 results about "Triethylsilane" patented technology

The invention relates to the technical field of organic synthesis, in particular to a method for constructing Orforglipron tetrahydropyran ring chirality through enzyme catalysis, which comprises the following steps: step S1, taking SM1 as a raw material, and carrying out hydrolysis resolution in a solvent, a buffer salt system and enzyme catalysis to obtain a chiral pure intermediate INT-1; step S2; performing ring closing on the INT-1 through Grignard reaction to synthesize a lactone intermediate; s3, carrying out Diball-H reduction, quenching, dichloromethane extraction and anhydrous sodium sulfate drying on the INT-4, and then reducing the INT-4 by using triethyl silane to obtain an intermediate INT3; step S4, coupling the INT-3 in the presence of a catalyst and a ligand to obtain an intermediate INT-4; step S5, carrying out deprotection and salification on the INT-4 to obtain an intermediate INT5; s6, closing an indole ring from INT5 to obtain a compound of which the general formula is A; chirality is constructed through enzyme catalysis, isomer impurities do not need to be split and separated through SFC when the chirality is constructed, the loss is reduced, the yield is increased, and a target product is obtained with high chiral selectivity; meanwhile, the cost is relatively reduced, and the cost is saved.

The present invention relates to the technical field of organic synthesis, and specifically relates to a method for constructing the chirality of a pyran ring in Orforglipron by means of enzymatic catalysis, the method comprising the following steps: step S1, by using SM1 and SM2 as starting materials, carrying out a reaction under the action of a palladium catalyst and a ligand to obtain INT-1; step S2, under the catalysis of Pd / C, subjecting INT-1 to double bond hydrogenation reduction to obtain INT-2; step S3, in the presence of a solvent, a buffer salt system and enzymatic catalysis, subjecting INT-2 to hydrolysis and resolution to obtain a chirally pure intermediate INT-3; step S4, subjecting INT-3 to a Grignard reaction for cyclization, so as to synthesize a lactone intermediate INT-4; and step S5, subjecting INT-4 to reduction by means of Dibal-H, quenching same, performing extraction with dichloromethane, drying same with anhydrous sodium sulfate, and then performing reduction by means of triethylsilane to obtain a compound of general formula A. In the present invention, the chirality is constructed by means of enzymatic catalysis without the need of SFC resolution for separating isomeric impurities during the construction of the chirality, thereby reducing losses and improving yield, obtaining the target product at high yield and high chiral selectivity, and further saving expenses and reducing costs.

The invention discloses a preparation method of 3-((1r, 3r, 5r, 7r)-adamantane-2-yl) propiolic acid. The preparation method provided by the invention comprises the following steps: (1) taking adamantanone as a starting raw material, and carrying out French reaction to prepare a compound 2; (2) the compound 2 is subjected to a dehydroxylation reaction under the action of boron trifluoride diethyl etherate and triethyl silane, and a compound 3 is prepared; and (3) carrying out hydrolysis reaction on the compound 3 under the action of LiOH to obtain a target product, namely 3-((1r, 3r, 5r, 7r)-adamantane-2-yl) propiolic acid. The preparation method disclosed by the invention is short in process route, simple and convenient to operate, mild in reaction condition, easy to control, high in yield, few in by-products, relatively low in cost and suitable for process amplification.

The invention relates to a green synthesis method of triphenylphosphine, which belongs to the technical field of organic synthesis, and comprises the following steps: Step 1: adding a solvent, benzene and a catalyst aluminum trichloride into a reaction flask, heating to 25-30 DEG C, dropwise adding phosphorus oxychloride, after addition, carrying out heat preservation reaction, and after the reaction is finished, cooling to room temperature to obtain a reaction product; the heat preservation temperature is 25-30 DEG C, and the heat preservation time is 3-4 hours; 2, after the reaction is finished, water is added for washing and layering, an organic phase is concentrated, the solvent is recycled, and triphenylphosphine oxide is obtained; 3, reducing the triphenylphosphine oxide in a solvent through a reducing agent to obtain triphenylphosphine, wherein the reducing agent is a triethyl silane / oxine copper reduction system; and Step 4, after the reaction is finished, cooling to room temperature, adding water for washing and layering, concentrating an organic phase, and recovering the solvent to obtain the triphenylphosphine. The synthesis method is safer and more environment-friendly, the greenization of the process is embodied, the safety and environmental protection pressure is greatly relieved, the technological process is simple, the yield is high, and the synthesis method is suitable for industrial large-scale production.

The invention discloses a preparation method of an LH-1801 key intermediate, and belongs to the field of medicine synthesis. The preparation method comprises the following steps: enabling SM1 and NBS to react in an acid solution to obtain a compound 1; catalyzing the compound 1 and NBS in an organic solvent in the presence of a catalyst to obtain a compound 2; catalyzing the compound 2 and thionyl chloride in the presence of a catalyst to obtain a compound 3; performing Friedel-Crafts reaction on the compound 3 and 2-ethylthiophene in an organic solvent under the catalysis of a catalyst to obtain a compound 4; reacting the compound 4 with triethyl silane and boron trifluoride diethyl etherate in an organic solvent to obtain a compound 5; reacting the compound 5 with a salt solvent in an organic solvent to obtain a compound 6; and finally, reacting the compound 6 with an alkali solvent in an organic solvent to obtain a compound 7, namely the LH-1801 intermediate. According to the method, 2-chloro-4-methyl benzoic acid is used as a starting material, the intermediate steps are simple and mild reactions, the operation difficulty is low, the reaction risk is low, and the method is suitable for industrial production.

The invention relates to the technical field of organic synthesis, in particular to a method for continuously producing canagliflozin by using a microchannel reactor. The production method comprises the following steps: reacting M1 and isopropyl magnesium chloride lithium chloride in a microreactor 1 to form an intermediate I; the reaction temperature is-10 DEG C to 10 DEG C; the reaction time is 15 to 45 seconds; reacting the intermediate I with the M2 in a microreactor 2 to form an intermediate II; the reaction time is 20 to 60 seconds; reacting the intermediate II, methanesulfonic acid and C1-C3 alcoholic solution in a microreactor 3 to form an intermediate III; the reaction time is 20 to 60 seconds; and reacting the intermediate III, triethyl silane and boron trifluoride diethyl etherate in a microreactor 4 for 5-10 seconds. The method solves the problems that the micro-channel reactor is easy to block and the product purity is not high.

The invention discloses a synthesis method of high-purity triethyl silane, and belongs to the technical field of organosilicon compound synthesis. The method solves the problems of low purity, poor stability and serious pollution of the existing synthesis method, sodium hydride and trimethyl borate are used as starting raw materials, a trimethoxy sodium borohydride solution is generated in situ under a low-temperature condition, then the trimethoxy sodium borohydride solution and accurately metered triethyl chlorosilane are subjected to a mild and controllable reduction reaction, and the high-purity triethyl chlorosilane is obtained. According to the method, the dependence of a traditional process on a noble metal catalyst or a highly toxic reducing agent is abandoned, the reaction safety is improved from the source, the complete reaction is promoted by adopting the composite catalyst, and the hydrophobic modified 3A molecular sieve is innovatively utilized for low-temperature adsorption purification, so that key impurities such as trace moisture and chloride ions can be efficiently removed; and finally, high-vacuum precise rectification is combined, so that a high-purity triethyl silane product can be obtained.

The application relates to the technical field of compound synthesis, and discloses an aromatic dipeptide functionalized mercapto compound, 3,5-di(triphenylmethylthio)benzoic acid is obtained by adding 3,5-di(methylmercapto)benzoic acid and pyridine into a solution of chloromethyl triphenylphosphonium, purifying after sufficient reaction; then the 3,5-di(triphenylmethylthio)benzoic acid is mixed with N-hydroxysuccinimide and dissolved in an organic solvent, EDC.HCl is added, purifying after sufficient reaction; then 2,5-dioxopyrrolidin-1-yl 3,5-bis(triphenylmethylthiomethyl)benzoate is obtained; then phenylalanine-tryptophan and triethylamine are added, purifying after sufficient reaction; then (3,5-bis(triphenylmethylthiomethyl)benzoyl)tryptophylphenylalanine is obtained; then trifluoroacetic acid and triethylsilane are added, purifying after sufficient reaction; and finally the aromatic dipeptide functionalized mercapto compound is obtained. The aromatic dipeptide functionalized mercapto compound can quickly and effectively identify sodium and potassium ions, and has relatively low detection limit and relatively loose detection condition.

The invention relates to a synthetic method of 2-diphenylmethyl pyrrolidine or an acid salt of 2-diphenylmethyl pyrrolidine. In order to solve the problems of easy ring opening and low yield in the prior art, the invention provides a synthetic method of 2-diphenylmethyl pyrrolidine or an acid salt thereof, which comprises the following steps: in the presence of an alkaline reagent, performing amidation and esterification reaction on a compound pyrrole-2-formic acid as shown in a formula II and ethyl chloroformate in an ROH solvent to obtain a compound as shown in a formula III; r in the ROH solvent is alkyl; performing Grignard reaction with phenyl magnesium bromide to obtain a compound as shown in a formula IV; carrying out reduction reaction on the compound shown in the formula IV under the catalytic action of trifluoroacetic acid and triethyl silane to obtain a compound shown in a formula V; and carrying out hydrolysis reaction on the compound in the formula V under an alkaline condition to obtain the compound 2-diphenylmethylpyrrolidine in the formula I or the acid salt thereof. According to the method, ring-opening impurities can be effectively avoided, the yield is increased to 95% or above, and the purity reaches 99% or above.

The invention provides a preparation method of modified fiber aerogel, which comprises the following steps: carrying out electrostatic spinning on a spinning solution under the assistance of airflow to obtain a doped SiO2-ZrO2 nanofiber aerogel precursor; taking one or two of triaminopropyl triethyl silane and triaminopropyl methyl diethoxy silane to prepare a liquid silane aqueous solution; and depositing an organosilane polymeric membrane on the SiO2-ZrO2 doped nanofiber aerogel precursor by using a liquid silane aqueous solution through a low-temperature and low-pressure vapor deposition method to obtain the modified fiber aerogel. The high polymer fiber prepared by electrostatic spinning has a large amount of Si-OH, the group is uniformly spread on the surface of the fiber, and meanwhile, the existence of the group provides a reaction site for a subsequent gas phase reaction, so that the preparation of a fiber aerogel coating is realized in a low-pressure and low-temperature environment. The high temperature resistance and the mechanical property of the prepared super-uniform fiber coating are greatly improved.

The invention discloses a preparation method of fulvestrant, according to the preparation method, triphenyl halogenated methane is used as a hydroxyl protection reagent, more target products are generated during alkyl chain substitution through a steric effect, in addition, triethyl silane and boron trifluoride diethyl etherate are used for reducing carbonyl and removing protection at the same time, and the reaction conditions are simple and mild. Meanwhile, carbonyl and protecting groups are removed in the step, so that subsequent thioether bonds are not affected, the impurity amount is reduced, raw materials in the whole reaction route are cheap and easy to obtain, the preparation route is short, the overall molar yield reaches 65%, and a reference route is provided for industrial preparation of fulvestrant.

This utility model relates to the field of triethylsilane synthesis technology and discloses an apparatus for triethylsilane synthesis, comprising: a raw material storage component for storing synthesis raw materials; a mixing device for mixing the raw materials output from the raw material storage component; and a fixed-bed reactor filled with a catalyst. By providing the temperature required for the reaction, the mixed raw materials react with each other on the catalyst surface under certain pressure and temperature to generate the desired substance. This utility model provides a production apparatus for triethylsilane, which is a fully continuous process device including reaction and separation processes. This apparatus supports the production of triethylsilane from tetrahydrosilane and ethylene via fixed-bed catalytic reaction. The apparatus has a simple process, high atom utilization, simplified flow, no solvent use, low waste, and can achieve continuous and automated operation.

The present invention discloses a method for constructing a super-hydrophobic surface of an iron-based amorphous alloy coating and significantly improving its corrosion resistance, and relates to the field of surface engineering technology. The method comprises: S1, obtaining an iron-based amorphous coating by HVAF technology, S2, chemical etching treatment of the coating surface, S3, crosslinking of nano-TiO2 particles with a perfluorodecyltriethylsilane solution, and S4, modification of the coating surface. The method has the following advantages: (1) the coating after spraying has a natural roughness suitable for manufacturing a super-hydrophobic surface; (2) the surface treatment process is simple, efficient, and low in cost; (3) the composite of nanoparticles and perfluorodecyltriethylsilane not only realizes the construction of a super-hydrophobic surface nanostructure and the reduction of surface energy, but also has the function of filling the pore defects generated by the amorphous coating during the preparation process; (4) the coating has good super-hydrophobicity and self-cleaning properties, and at the same time exhibits significantly outstanding corrosion resistance.

This invention relates to the field of asymmetric catalytic hydrogenation, specifically to a method for preparing chiral chromone or chromane carboxylic acid compounds. The method involves preparing a chiral catalyst from a nickel compound and ligands. By controlling the combination of the nickel compound-ligand-solvent, enantioselective hydrogenation of the conjugated C=C bonds of the substrate chromone carboxylic acid compound is achieved, yielding the semi-reduced product chiral chromone carboxylic acid; or, further, the carbonyl group is reduced, and carbonyl reduction and dehydroxylation reactions are carried out at room temperature under trifluoroacetic acid and triethylsilane conditions to obtain the fully reduced product chiral chromane carboxylic acid. The catalytic system of this invention is simple to construct, and the selectivity can be controlled by the solvent system. It maintains high conversion and excellent enantioselectivity even under high S / C conditions, making it suitable for the efficient preparation of chiral chromone / chromane skeletal carboxylic acid compounds.

The invention relates to the technical field of synthesis of triethyl silane, and discloses a synthesis method of triethyl silane, which comprises the following steps: taking tetrahydride and ethylene as starting materials, and generating triethyl silane on a fixed bed reactor under the catalytic action of a catalyst. The technical process is simple, the equipment investment is low, no solvent is needed, purification is convenient, the front fraction diethylsilane can be mechanically applied to the production process, the material use efficiency is improved to the maximum extent, and tetraethylsilane can also be sold as a byproduct after being purified.

The invention provides an alkyl uracil derivative and a preparation method and application thereof, and relates to the technical field of organic synthesis.The preparation method comprises the following steps that a uracil analogue and olefin are subjected to a hydrogenation alkylation reaction under the action of an iron catalyst and a hydrogen source, and the alkyl uracil derivative is obtained; the iron catalyst comprises at least one of iron nitrate nonahydrate, ferrous nitrate, ferric chloride, ferrous chloride, ferric sulfate and ferric oxalate; the hydrogen source comprises at least one of sodium borohydride, lithium borohydride, lithium aluminum hydride, triphenyl silicon, triethyl silicon and borane. According to the present invention, the olefin is adopted as the alkyl raw material, the pre-functionalization is not required, the specific catalyst and the specific hydrogen source are combined, the hydrogenation alkylation reaction of the olefin and the uracil analogue is successfully achieved, and the technical effect of constructing a series of alkyl uracil derivatives is achieved. According to the invention, the reaction can be carried out at room temperature without light and heat conditions, the reaction time is short, and the functional group tolerance is better.

The present invention discloses a method for synthesizing N-trifluoromethylsulfonamide compounds. The method uses aromatic isothiocyanates as starting materials and utilizes a series of reagents, including silver fluoride, triethylsilane, p-toluene thionyl chloride, m-chloroperbenzoic acid, and potassium fluoride, to synthesize N-trifluoromethylsulfonamide compounds through a multi-step reaction. The present invention introduces a trifluoromethyl group into the sulfonamide structure, while maintaining mild reaction conditions and utilizing a wide range of raw material sources.

The invention discloses a novel synthesis method of 5-aryl-3-alkyl pyrazolo [1, 5-a] pyridine, which comprises the following specific synthesis steps: adding an X2 donor compound into a solvent containing a compound SM at 0-5 DEG C, stirring at 0-5 DEG C for complete reaction, and performing post-treatment to obtain a compound 1; adding the compound 1 into a solvent, adding an organic metal reagent at 0-5 DEG C in a protective atmosphere, stirring at room temperature for complete reaction, and performing post-treatment to obtain a compound 2; dissolving the compound 2 and triethyl silane in a solvent, adding trifluoroacetic acid, stirring to react completely, and performing post-treatment to obtain a compound 3; under a protective atmosphere, dissolving the compound 3, Pd (dppf) Cl2, B2Pin2 and alkali in an organic solvent, and carrying out reflux stirring reaction completely to obtain a compound 4; and under a protective atmosphere, adding water, Pd (dppf) Cl2 and ArX into the reaction liquid containing the compound 4, carrying out reflux stirring to completely react, and carrying out post-treatment on the reaction liquid to obtain a target compound 5. The method is short in step, easy to operate in each step, high in yield and suitable for large-scale amplification.

The present invention provides a cyanide-free electrolyte for hard gold electroforming and a preparation process thereof, belonging to the technical field of gold plating processes; the preparation process comprises the following steps: adding 4-dimethylaminopyridine to react and prepare additive A; adding lithium tert-butoxide to react and prepare additive B; preparing an AuCl3 solution; dissolving 5,5-dimethylhydantoin and adding each component. The present invention is prepared by stirring and mixing N-acetyl-L-cysteine, triphenylmethanol and dichloromethane and mixing them with trifluoroacetic acid; after vacuum distillation, purification and elution, triethylamine, 4-dimethylaminopyridine and acetic anhydride are added to react, and trifluoroacetic acid and triethylsilane are added to react to prepare additive A. After adding the cyanide-free electrolyte, during the gold electroplating process, the additive A can effectively promote the formation of crystal nuclei, prevent excessive grain growth, and promote gold grain refinement. The fine and evenly distributed grain structure can significantly improve the hardness and wear resistance of the coating.

The invention discloses a method for synthesizing an allyl reagent by alkali-promoted silanization of 1, 3-diene, and relates to the technical field of synthesis of organic compounds, the method comprises the following steps: in an argon atmosphere, synthesizing methyl sulfide of 1, 3-butadiene through bis (methylthio) trimethylsilyl methane and cinnamyl aldehyde compounds; the preparation method comprises the following steps: reacting bis (pinacol) diboron and triethyl silane under an oil bath condition to prepare triethyl silicon-based boronic acid pinacol ester; the preparation method comprises the following steps: mixing sodium tert-butoxide, methyl sulfide of 1, 3-butadiene, triethylsilylboronic acid pinacol ester and tetrahydrofuran, and heating to react, so as to prepare the disilylated allyl compound. The method provides a first technology for synthesizing the allyl reagent through silanization of 1, 3-diene by using alkali under the condition of non-metal catalysis, and solves the problems of environmental pollution, high cost and the like caused by the use of traditional transition metal catalysis in the synthesis of the existing allyl silane reagent.

The application discloses a preparation method of an aromatic amine compound. The aromatic amine compound is obtained from an aromatic nitro compound in a triethylsilane and iodine element system at room temperature through one-step reaction. The application is easy to prepare under the premise of obtaining a good yield and is simple in overall step operation and mild in reaction process.

Embodiments are directed to a method of making an olefin-based polymer by free-radical polymerization in a reactor system. The method includes initiating a free-radical polymerization of an olefin-based monomer, propagating growth of the olefin-based polymer during continued free-radical polymerization of the olefin-based monomer, and adding to the reactor system a chain transfer agent that terminates the growth of the olefin-based polymer. The chain transfer agent includes a silane. Examples of suitable silanes are: triethylsilane, diethylmethylsilane, tris(trimethylsilyl)silane, n-butylsilane, dimethylphenylsilane, phenylsilane, chlorodimethylsilane, diisopropylaminosilane, 1,2-bis(dimethylsilyl) benzene, 1,3-bis(dimethylsilyl) benzene, 1,4-bis(dimethylsilyl)benzene, 1,1, 3,3-tetramethyldisiloxane, trimethylsilane, (trimethylsilyl)dimethylsilane, and bis(trimethylsilyl)methylsilane.

The invention relates to the technical field of nano materials, and particularly discloses a preparation process of nano silicon dioxide coated spherical wax micro powder particles. The preparation process comprises the following steps: weighing raw materials; the preparation method comprises the following steps: blending deionized water, absolute ethyl alcohol and ethidene diamine according to a ratio, adding an organic silicon source under normal temperature and stirring, and uniformly stirring to obtain silica sol; wetting the spherical wax micro-powder particles with hydrogen peroxide, adding vinyltriethylsilane and butyltin dilaurate, uniformly stirring, heating to a temperature below the melting point and above the glass transition temperature of the spherical wax micro-powder particles, and then cooling to normal temperature to obtain pretreated wax micro-powder particles; and adding the pretreated wax micro powder particles into silica sol under stirring, uniformly dispersing, grinding to obtain a thick slurry-shaped dispersion, carrying out solid-liquid separation, and drying to obtain the spherical wax micro powder particles coated with nano silicon dioxide. According to the method, the stability of the coating layer of the spherical wax micro powder particles coated with the nano silicon dioxide can be improved.

The invention discloses a normal-pressure synthesis method of a carfilzomib intermediate, which is characterized in that the intermediate ASC007-I reacts in the presence of lower alcohol, palladium on carbon and a hydrogen source to obtain ASC007-II, and the hydrogen source is one of zinc powder and hydrochloric acid, methyl formate and hydrochloric acid and triethyl silane. Methyl formate / hydrochloric acid, zinc powder / hydrochloric acid and triethyl silane are used as hydrogen sources, under an alcohol solvent system, catalytic debenzylation is carried out through palladium-carbon catalysis, the compound ASC007-II is generated, pressurization and hydrogen introduction are not needed in the reaction, the problems that the reaction is high in equipment requirement and not suitable for industrial production are solved, the reaction conditions are milder, the process controllability is high, the yield is high, and the method is suitable for industrial production. The industrial production is facilitated.