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132 results about "Triethylsilane" patented technology

Triethylsilane is the organosilicon compound with the formula (C₂H₅)₃SiH. It is a trialkylsilicon hydride compound. The Si-H bond is highly reactive. This colorless liquid is used in organic synthesis as a reducing agent and as a precursor to silyl ethers.

Trimethylgallium, a method for producing the same and a gallium nitride thin film grown from the trimethylgallium

The present invention provides a trimethylgallium which has less than 0.1 ppm of a total organic silicon compound content; and a method for producing the trimethylgallium comprises hydrolyzing trimethylaluminum as a raw material, extracting organic silicon compound contained with a solvent, quantifying methyltriethylsilane by a Gas Chromatography-Mass Spectrometry, selecting a trimethylaluminum having less than 0.5 ppm of methyltriethylsilane content for the raw material, purifying by distillation, followed by reaction with gallium chloride and then distilling the reactant solution to obtain the trimethylgallium.
Owner:SUMITOMO CHEM CO LTD

Method for preparing 2-P-octyl-phenenl-2-amino-propanediol hydrochloride

The invention offers 2-amphi capryl phenethyl-2-amino group propylene glycol hydrochloride preparation method. It includes the following steps: doing Friedel-Crafts reaction for styrene and capryl chloride to produce amphi capryl styrene; doing Michael addition reaction with kharophen diethyl malonate under alkali action to produce 2-amphi capryl phenethyl-2-kharophen diethyl malonate; reacting with triethyl silane to produce 2-amphi capryl phenethyl-2-kharophen diethyl malonate; reducing and hydrolyzing to produce 2-amphi capryl phenethyl-2-amino group propylene glycol; acidifying with hydrochloric acid to produce salt. It has the advantages of simple line, low cost, short period, little pollution, and high yield. It also offers the intermediate compound preparation method.
Owner:NANJING YOKO PHARMA GRP CO LTD

Preparation method of improved avibactam sodium intermediate compound

The invention belongs to the technical field of medical chemistry and particularly relates to a preparation method of beta-lactamase inhibitor drug avibactam sodium and an intermediate of beta-lactamase inhibitor drug avibactam sodium. Triethyl-silane is adopted to realize benzyl removal, hydrogenation catalysis operation in the prior art is omitted, the reaction condition is milder, safety risk is reduced, the product yield and the purity are greatly improved, and the preparation method is more suitable for large-scale production.
Owner:QILU PHARMA HAINAN +1

Method for asymmetrically synthesizing glabridin with optical purity under catalysis of ruthenium compound

The invention relates to a method for asymmetrically synthesizing glabridin with optical purity under catalysis of a ruthenium compound. The method comprises the following steps: 1) taking isoflavoneprotected by a protection group as a raw material and carrying out dynamic kinetic asymmetric hydrogen transfer reaction under the catalysis effect of a ruthenium trichloride compound and the action of an acid-alkali buffering system to obtain chiral isoflavol with an absolute configuration being (3R, 4R); 2) removing hydroxyl of the chiral isoflavol under the action of triethylsilane and trifluoroacetic acid to obtain a product with an absolute configuration being (R); 3) removing a protection group of the product with the configuration being (R) in step 2) under an acidic or alkaline condition to obtain the glabridin with the configuration (R) and the optical purity. The method provided by the invention can be used for synthesizing the glabridin with the optical purity in a high-yield and high-stereoselectivity manner; the obtained product is completely the same as that of the glabridin extracted from glycyrrhiza glabra and can be used for replacing the glabridin derived from naturalplants to be industrially applied.
Owner:烟台六谛医药科技有限公司 +2

Preparation method of silodosin intermediate

The invention discloses a preparation method of a silodosin intermediate. The preparation method comprises the following steps that in an organic solvent, under the action of lewis acid, friedel-crafts acylation reaction occurs between a compound 2 and a compound 3, so as to obtain a compound 4, wherein the lewis acid is one of or more of zinc trifluoromethanesulfonate, bismuth trifluoromethanesulfonate, scandium trifluoromethanesulfonate and aluminum trichloride; under the action of organic acid or boron trifluoride ether complex, the compound 4 reacts with triethyl silicane, so as to obtain a compound 5; the compound 5 reacts with sodium azide, so as to obtain a compound 6; under the action of catalysts, the compound 6 reacts with di-tert-butyl dicarbonate ester and hydrogen, so as to obtain a compound 7; under an acidic condition, the deamination protective reaction of the compound 7 occurs, so as to obtain a compound 8; the compound 8 reacts with L-tartaric acid, so as to obtain a compound 1, namely the silodosin intermediate. The preparation method of the silodosin intermediate has the advantages of simplicity, economy and mild reaction conditions, and chiral resolution is not needed.
Owner:ZHEJIANG TIANYU PHARMA

Preparation method of gold nano-composite targeting drug delivery system

The invention discloses a preparation method of a gold nano-composite targeting drug delivery system. The preparation method comprises the following steps: sequentially adding a chloroauric acid solution and a silver nitrate solution into a hexadecyl ammonium bromide solution, mixing uniformly, then sequentially adding an ascorbic acid solution and a gold nano-particle seed solution, and centrifuging to obtain a gold nano-bar; adding ethyl orthosilicate to obtain a mesoporous silicon oxide nano-material; adding 3-aminopropyl triethylsilane to obtain aminated GNRs@mSiO2; adding a thionyl chloride solution of melphalan to obtain aminated GNRs@mSiO2-MEL; and adding HA-RGD to obtain GNRs@mSiO2-HA-RGD-MEL. According to the preparation method, gold nano-particles with an effect of photothermal therapy are effectively combined with an anti-cancer drug, namely melphalan, thereby realizing combined therapy of tumor thermotherapy and chemotherapy and increasing the therapeutic effect; and by utilizing mesoporous silicon oxide ducts for efficiently loading drugs, the drug loading capacity can be increased.
Owner:WUHAN UNIV OF TECH

Block boron carbide-silicon carbide composite aerogel preparation method

The invention relates to a block boron carbide-silicon carbide composite aerogel preparation method. The method includes: stirring nano boron carbide powder, resorcinol, formaldehyde, 3-aminopropyl triethyl silicane, absolute ethyl alcohol and deionized water according to a mole ratio to obtain faint yellow composite sol solution, and standing to obtain wet gel; subjecting the wet gel to solvent replacement, drying the wet gel according to a CO2 supercritical drying technique to obtain a boron carbide-silicon carbide precursor, and adopting a carbon thermal reduction technique in an inert atmosphere to obtain block boron carbide-silicon carbide composite aerogel. The block boron carbide-silicon carbide composite aerogel prepared according to the method has advantages of high specific surface, low density, high porosity, high temperature resistance and the like, a technical process is simple and easy in operation, and preparation of the block boron carbide-silicon carbide composite aerogel hopefully has a promising application prospect in fields of chemical equipment, high-temperature kilns and the like.
Owner:NANJING UNIV OF TECH

Preparation method of high temperature-resistant boron carbide-silicon carbide compound aerogel

The invention relates to a preparation method of a high temperature-resistant boron carbide-silicon carbide compound aerogel. The method comprises taking absolute ethyl alcohol and deionized water assolvent, mixing a preferable boron source with m-dihydroxybenzene, formaldehyde and 3-aminopropyl triethyl silane at a certain molar ratio to obtain a solution, namely, light yellow compound gel; performing aging and solvent replacement on the wet gel and then drying the wet gel through the supercritical drying technology to obtain a boron carbide-silicon carbide precursor, and under protection ofinert gas and through carbon thermal reduction, obtaining the high temperature-resistant boron carbide-silicon carbide compound aerogel. The preparation method of the high temperature-resistant boroncarbide-silicon carbide compound aerogel is simple and reliable in preparation process and rich and simple in raw materials; the prepared high temperature-resistant boron carbide-silicon carbide compound aerogel can be widely applied to the fields such as chemical equipment and high-temperature kiln.
Owner:NANJING TECH UNIV

Preparation method of levo-5-hydroxytryptophan

The invention provides a preparation method of levo-5-hydroxytryptophan. The method comprises the following steps: performing methyl esterification / ethyl esterification on L-tryptophan to obtain L-tryptophan methyl / ethyl ester hydrochloride, performing dehydrochlorination under the alkaline condition to obtain L-tryptophan methyl / ethyl ester, performing acetylation to obtain N-acetyl-L-tryptophanmethyl / ethyl ester, reducing an indole ring under a triethylsilane-trifluoroacetic acid reduction system, oxidizing 1-position nitrogen of the indole ring under a sodium tungstate-30% hydrogen peroxide system, finally removing acetyl protection group to obtain levo-5-hydroxytryptophan under the acidic condition, further cooling and crystallizing, then enabling mother liquor to pass through a macroporous adsorption resin column, performing concentration, cooling and crystallization, and combining obtained levo-5-hydroxytryptophan crystals. The process has the advantages of being low in price of raw materials, being easy to obtain the raw materials, being simple in reaction operation, being high in yield, being good in product quality, being low in environmental pollution and the like, and is suitable for industrial large-scale production, the purity of the obtained product can achieve 99.2%, and the total yield is above 45%.
Owner:FOSHAN PRIZEN MEDICAL TECH

Cabazitaxel intermediate as well as preparation method and application thereof

The invention discloses a cabazitaxel intermediate as well as a preparation method and an application thereof. The intermediate has a chemical structure formula shown as formula I shown in the description, and TES in the formula is the abbreviation of triethylsilane. The preparation method of the intermediate comprises a step B or a step A and the step B in the following synthetic route shown in the description, wherein the step A means that the compound of a formula 1 is subjected to a methylation reaction with a methylation agent for preparation of the compound of a formula 2; and the step B means that the compound of the formula 2 is subjected to a condensation reaction with the compound of a formula 3 for preparation of the intermediate I. The intermediate is subjected to hydrolysis under an acidic condition for removing the triethylsilane protective group, and thus cabazitaxel is prepared. According to the technical scheme, high-purity cabazitaxel can be synthesized by utilizing cheap and easily-available raw materials and with a low cost, large-scale industrialized production requirement on cabazitaxel is satisfied, and the preparation method is applicable to industrial application and has practical value.
Owner:SHANGHAI ACEBRIGHT PHARMA CO LTD +1

Making method of anti-sticking polyurethane elastomer lining plate

A making method of an anti-sticking polyurethane elastomer lining plate comprises the following steps: putting polyester polyol in a sand mill, adding molybdenum disulfide micropowder and colloidal graphite micropowder, dispersing, placing the obtained mixture in a reaction kettle, heating, carrying out vacuum pumping stirring dehydration, cooling, adding toluene diisocyanate and methyl diphenylene diisocyanate, heating, carrying out a polymerization reaction, and defoaming to prepare a polyurethane prepolymer; adding 1H,1H,7H-dodecafluoro-1-heptanol, a TDI-100 compound, triethyl silane and polytrifluoropropylmethylsiloxane, stirring, and carrying out heating reacting and defoaming to obtain a polyurethane prepolymer mixture containing fluorine and silicon; and heating 3,3'-dichloro-4,4'-diaminodibenzyl methane for melting, mixing with the polyurethane prepolymer mixture containing fluorine and silicon, carrying out cast molding by a casting machine, and carrying out release vulcanizing to make the anti-sticking polyurethane elastomer lining plate. The lining plate has the advantages of seismic resistance, low noise, sticking resistance, wear resistance and the like, and can satisfy the requirements of the lining plate in the material transportation process of all industries.
Owner:太原英可奥笔墨科技有限公司

Method for preparing 2-amino-2-[2-(4-alkyl phenyl) ethyl]-1,3-propanediol hydrochloride

The invention discloses a method for preparing 2-amino-2-[2-(4-alkyl phenyl) ethyl]-1,3-propanediol hydrochloride. The method comprises the following steps of: firstly, enabling a compound shown as a formula (II) and diethyl acetamidomalonate to be subjected to a condensation reaction under the action of a catalyst to obtain a compound shown as a formula (III); enabling the compound shown as the formula (III) as well as triethyl silane and titanium tetrachloride to be subjected to a reaction to prepare a compound (IV); then, continuously enabling the compound (IV) as well as lithium aluminum hydride and acetic anhydride to be subjected to a reaction to prepare a compound (V); and finally, enabling the compound (V) as well as lithium hydroxide and concentrated hydrochloric acid to be subjected to a reaction to obtain a compound shown as the formula (I). A midbody (III) prepared by using the method provided by the invention has enough purity and high yield up to over 95%, and purification through column chromatography is not needed in the reaction process, so that the next reaction can be directly carried out. The final target compound is synthesized by using easily purchased raw materials in a short way, and the method is short in production period, high in yield, mild in reaction condition, simple and feasible and suitable for industrial production.
Owner:NANJING HUAWE MEDICINE TECH DEV +1

Method for preparing canagliflozin intermediate 2-(4-fluorophenyl)-5-[(5-halogen-2-methylphenyl)methyl]thiophene

The invention discloses a method for preparing canagliflozin intermediate 2-(4-fluorophenyl)-5-[(5-halogen-2-methylphenyl)methyl]thiophene. A compound, which is represented as formula II, is subjected to a reduction reaction, catalyzed by a protonic acid or a Lewis acid, through a metal borohydride to obtain a compound canagliflozin intermediate I. The intermediate I is a key intermediate for preparing a diabetes drug canagliflozin. According to the method in the invention, triethyl silicane, which is high in dangerousness and has a pungent smell, is replaced by the metal borohydride. The method is safer in technology, is environment-friendly, is low in cost and is suitable for large-scale production.
Owner:SHANGHAI FANGNAN PHARMA

Method for preparing lubiprostone compound

The invention relates to a method for preparing lubiprostone. The method comprises the following steps: by taking triethyl silicane as a hydrogen source, and taking palladium carbon or palladium hydroxide as a catalyst, performing catalytic transfer hydrogenation, removing the protecting groups, and reducing double bonds, thereby obtaining the product. Compared with a conventional catalytic hydrogenation reaction at present, the method has the advantages of simplicity in operation, mild reaction conditions, high yield and high purity, the reaction time and reaction period are obviously shortened, the production efficiency is greatly improved, the requirements on reaction equipment are reduced, and the method is suitable for industrial production.
Owner:QILU PHARMA CO LTD

Method for preparing high purity Empagliflozin

The present invention provides an improved method for preparing high purity Empagliflozin, the method includes the following steps: step a. under the protection of nitrogen, performing reaction of compounds 1 and 2 to obtain a compound 3; step b. adding the compound 3 into a reactor, adding methanol, dropwise adding concentrated hydrochloric acid, stirring, dissolving, clarifying, and performing reaction at room temperatur to obtain a compound 4; step c. adding dropwise an acetonitrile and dichloromethane solution of the compound 4 to an aluminium chloride, triethyl silicane, acetonitrile and dichloromethane solution for reaction, after completion of the reaction, adding water for quenching the reaction, stirring until a solid is precipitated, filtering by suction, and collecting a filter cake to obtain a crude product of compound 5, namely Empagliflozin; and d. refining the crude product. The method is suitable for industrial production,and can be used for the preparation of the high purity Empagliflozin.
Owner:YANGTZE RIVER PHARMA GRP BEIJING HAIYAN PHARMA +1

Synthetic method of dapagliflozin

Disclosed is a synthesis method of dapagliflozin. The method includes providing a microreactor having at least 4 reaction units in series, delivering a 5-bromo-2-chloro-4'-ethoxydiphenylmethane solution and an alkyllithium solution into a first reaction unit and controlling the reaction temperature in the first reaction unit to be -5 to -40 DEG C; after the reaction is completed, making a reactionsolution flow into a second reaction unit, and delivering trimethylsilyl protected gluconolactone or a solution thereof to the second reaction unit; after the reaction is completed, making a reactionsolution flow into a third reaction unit and delivering a mixed solution of methanol and methane sulfonic acid to the third reaction unit; making a reaction solution flow into a fourth reaction unitafter the reaction is completed and delivering a mixed solution of boron trifluoride diethyl etherate and Triethylsilane into the fourth reaction unit.
Owner:SHANDONG HIMILE CHEM TECH

Method for preparing triethyl silicane

The invention belongs to the field of the preparation of medicinal intermediates, and particularly relates to a method for preparing triethyl silicane. The method comprises the following steps of: performing a condensation reaction of trichlorosilane, halothane and magnesium powder in an alkane or arene organic solvent containing an ether catalyst, and purifying a reaction production to obtain the triethyl silicane. By the method for preparing the triethyl silicane, the obtained product has fewer impurities, and the product content is over 99 percent; and the preparation method has low cost, less pollution and mild reaction condition, is easy and convenient to operate, and is convenient for industrial production.
Owner:河南豫辰药业股份有限公司

Modified graphene enhanced waterborne FEVE fluorine-carbon flexible protection paint and coating

The invention discloses a modified graphene enhanced waterborne FEVE fluorine-carbon flexible protection paint. The modified graphene enhanced waterborne FEVE fluorine-carbon flexible protection paintis prepared from waterborne FEVE fluorine-carbon resin, a low-surface-energy auxiliary agent, a curing agent, a diluent and a grafting modified graphene function filler. According to the modified graphene enhanced waterborne FEVE fluorine-carbon flexible protection paint, through a silane coupling agent gamma-aminopropyl triethyl silicane, graphene is subjected to grafting modification, and the wettability of the graphene is effectively improved, so that the graphene is uniformly dispersed in a paint system; the grafting-modified graphene of a flaky structure is uniformly dispersed, stacked layer by layer and staggered in the waterborne FEVE fluorine-carbon resin to form a tight physical shielding structure, and water molecules and atmospheric corrosion mediums are effectively isolated from permeating a circuit board substrate or being diffused into the circuit board substrate; meanwhile, through the further combination of excellent low surface energy and hydrophobic properties of thefluororesin, the prepared protection paint has the functions of resisting water, dampness and salt-spray corrosion, and it is guaranteed that the protection paint has high reliability under extreme working conditions of high temperature, high humidity and high salt-spray corrosion.
Owner:NORTH CHINA UNIVERSITY OF TECHNOLOGY

Organic/inorganic hybrid nanometer porous anti-reflection coating

The invention discloses an organic / inorganic hybrid nanometer porous anti-reflection coating layer; the organic / inorganic hybrid nanometer porous anti-reflection coating layer, with the thickness of 42.5-162.8nm, porosity of 23.2%-56.9% and aperture of 5-10nm, is gained through a sol-gel process by taking poly-(methyl methacrylate-b- methacryloxypropyltriethoxysilane) as precursor or through the sol-gel process by taking the mixture of the poly-(methyl methacrylate-b-methacryloxypropyltriethoxysilane) and tetraethyl orthosilicate; the invention takes the micro-phase morphology of the block copolymer after the micro-phase separation as a template so as to prepare the organic / inorganic hybrid nanometer porous anti-reflection coating layer; the aperture size is easy to be controlled; furthermore, the distribution of the aperture is uniform, and the basic framework of the anti-reflection layer has Si-O-Si structure; the organic / inorganic hybrid nanometer porous anti-reflection coating layer has excellent mechanical performance, creasing resistance and friction resistance, is rich in Si-OH functional group and can effectively solve the adhesion problem caused by anti-reflection coating layers and various substrates prepared by the prior art.
Owner:ZHEJIANG UNIV

Preparation method for canagliflozin

The invention relates to a novel synthesis method for 1-(Beta-D-glucopyranosyl)-4-methyl-3-[5-(4-fluorophenyl)-2-thienylmethyl]benzene (canagliflozin). 2-(4-fluorophenyl)-5-[(5-halogeno-2-methylphenyl)methyl]thiophene and 2,3,4,6-tetrakis-O-(trimethylsilyl)-D-glucono-1,5-lactone are dissolved in organic solvent and carry out condensation reaction under the catalysis of a metallic lithium derivative, and thereby intermediate (II) is produced; the intermediate (II) undergoes catalytic hydrogenation reaction, so that intermediate (III) is further produced, and finally, compound (I), namely the canagliflozin is obtained by acidification hydrolysis. Because the preparation method disclosed by the invention replaces a virulent BF3 / triethyl silicane reduction system with the environment-friendly catalytic hydrogenation technique, the preparation method is technically safer, environment-friendly, low in cost and more suitable for industrial production.
Owner:SHOUGUANG FUKANG PHARMA

Carboxylic acid betaine type fluorine-containing compound as well as synthesis method and application thereof

The invention relates to a carboxylic acid betaine type fluorine-containing compound as well as a synthesis method and application thereof. A fluorinated tertiary amine compound as an initial raw material is reacted with tert-butyl bromoacetate to obtain a tert-butyl-protected quaternary ammonium salt product; the tert-butyl-protected quaternary ammonium salt product and triethyl silane are dissolved in anhydrous DCM, trifluoroacetic acid is dropwise added under an ice bath condition, the reaction is continued after the mixture is recovered to the room temperature, reduced pressure distillation is performed to remove a solvent and the trifluoroacetic acid, a product is dissolved by using a hydrochloric acid solution, and then is subjected to freeze-drying, the residual trifluoroacetic acidis removed by replacement, and the carboxylic acid betaine type fluorine-containing compound is finally obtained. The preparation method disclosed by the invention can be used for preparing a fluorinated polymer, the preparation method is simple, the yield is high, the separation is easy, and the purity is high. The compound contains a plurality of chemical active groups such as hydroxyl, amino,carboxyl, acetenyl, azido, and sulfydryl, can be used for labeling a drug, a polymer, a nanocarrier and an implant material, and satisfies the requirements of 19F MRI probe development.
Owner:INST OF BIOMEDICAL ENG CHINESE ACAD OF MEDICAL SCI

Compound and preparation method and application thereof

InactiveCN106279072AEfficient preparationThe reaction mechanism is clearOrganic chemistryImpurityHplc mass spectrometry
The invention provides a compound shown in the formula I and a preparation method thereof and a method for detecting Gliflozin medicine through high performance liquid chromatography. According to the preparation method, 3,5,6-tribenzyl-D-glucofuranose serves as a raw material, a methylation reaction, a benzyl substitution reaction, demethylating and ketalation are carried out, 3,5,6-tribenzyl-D-glucofuranose and a halide intermediate are subjected to a nucleophilic addition, the material makes contact with triethyl silicane and boron trifluoride diethyl etherate, finally, the material makes contact with ethanethiol and boron trifluoride diethyl etherate, and the target impurity product can be obtained. By means of the method, directional preparation is achieved for synthesis of the target product; the target product provides a reliable impurity reference substance for quality research and impurity quantitative control of industrially-produced Gliflozin series diabetes treatment medicine products. The formula I is shown in the specification.
Owner:WATERSTONE PHARMA WUHAN

The method for making candixatan ester and intermediates thereof

The method for making candixatan ester and intermediates thereof and a compound of formula III, wherein R1 is triphenylmethyl, methxoycarbonyl, ethoxycarbonyl, tert-butoxycarbonyl, benzoxycarbonyl, trimethylsilane, triethylsliane or tritertbutylsilane protect group, and R2 is triphenylmethyl, methxoycarbonyl, ethoxycarbonyl, tert-butoxycarbonyl, benzoxycarbonyl, trimethylsilane, triethylsliane ortritertbutylsilane protect group. The method for making candixatan ester by the said compound of formula III is also provided. The invention is a completely new synthesis route of candixatan ester which is shorter than ever, and the raw material is easily obtained, and the operation is simple. The new synthesis route of candixatan ester of the invention shortens the reaction route and simplifies the operation procedure. Furthermore, the new synthesis route of candixatan ester of the invention avoids the use of organo-tin and nitrine compounds, and which is safety and protects the environment.
Owner:SUZHOU VIGONVITA LIFE SCIENCES CO LTD

Introduction of alkyl substituents to aromatic compounds

InactiveUS20180065904A1Mercapto/sulfide group formation/introductionOrganic reductionThioenolElectrophilic aromatic substitution
Novel selective synthesis route to introduce primary alkyl groups on aromatic compounds is disclosed. The synthesis route is based on electrophilic aromatic substitutions of thionium ion species that are generated in-situ from aldehydes and thiols, affording benzyl sulfide that can be reduced with triethylsilane.
Owner:B G NEGEV TECH & APPL LTD

Biobased silicon-containing alternating EP rubber and preparation method thereof

TThe invention relates to a preparation method of biobased silicon-containing alternating EP rubber. Triethylsilane is used as a modifier, and a hydrosilation reaction is carried out for modification of gutta-percha. The triethylsilane modification reaction is carried out for modification of gutta-percha, the method can be carried out in a solution at a normal pressure, the operation is simple, the method has low requirements for equipment, and the method is easy to amplified and promoted. The modified rubber has strictly alternative ethylene and propylene, in the prerequisite that aging resistance and weatherability are not reduced, a reactive group is introduced to a gutta-percha main chain, and possibilities are provided for further modification. Compared with original gutta-percha elastomer, the structure has excellent interface compatibility as well as high moisture and slip resistance.
Owner:BEIJING UNIV OF CHEM TECH

Method for producing protein chip

Substantially, the invention is a method for fixing active protein molecules on surface of silicon, applicable to preparation of DNA chip and protein chip, belonging to area of biologic sensing technique. Characters of the invention are as follows. First, standard semiconductor technology is utilized to clean and oxidate silicon slice in high temperature. Next, silicon surface is treated by using gamma - amido - propyl - triethyl silane (gamma-APTES). Then, graph in nano size is etched on silicon surface by using nano etching technique of atomic force microscope (ATM). Finally, the silicon slice with prepared Nano graph is immersed into solution of protein. Thus, protein molecules are fixed on not etched silicon surface, and there is no protein molecule on the etched silicon surface. Advantages of the invention are: ensuring active of protein molecules effectively, and superhigh integration level of protein molecules.
Owner:SHANGHAI UNIV

Synthesis method of (R)-2-(2, 5-difluorophenyl) pyrrolidine

The invention belongs to the technical field of chemical pharmacy, and relates to a synthetic method of (R)-2-(2, 5-difluorophenyl)pyrrolidine. The synthesis method comprises the following steps: (1) carrying out dehydration condensation reaction on a compound as shown in a formula 1 and a chiral induction reagent (R) tert-butylsulfinamide to obtain a compound as shown in a formula 2; (2) carrying out addition reaction on the compound in the formula 2 and a Grignard reagent to obtain a compound in a formula 3; (3) carrying out a reduction / cyclization reaction on the compound shown in the formula 3, trifluoroacetic acid and triethylsilane to obtain a compound shown in a formula 4; (4) splitting the compound shown in the formula 4 by (D)-malic acid to obtain the (R)-2-(2, 5-difluorophenyl) pyrrolidine*D malate compound with EE being greater than 98% shown in the formula 5; and (5) dissociating the compound in the formula 5 with a sodium hydroxide solution to obtain (R)-2-(2, 5-difluorophenyl) pyrrolidine. By utilizing the synthetic method of (R)-2-(2,5-difluorophenyl)pyrrolidine, the cost is low, the optical purity is high, the subsequent separation process is simplified, the raw materials are easy to obtain, the process conditions are mild, and the synthetic method is suitable for synthesizing (R)-2-(2, 5-difluorophenyl) pyrrolidine in large-scale production.
Owner:北京蓝博特科技有限公司

Phospholipid compound and preparation method thereof

The invention discloses a phospholipid compound and a preparation method thereof. The structural general formula of the phospholipid compound is shown in the specification. In the formula, m is a positive integer from 2 to 10, and n is a positive integer from 7 to 15. The compound contains a disulfide bond easy to break and can be quickly broken and degraded in a reducing medium. The method comprises the following steps: (1) dissolving triphenylmethyl protected mercapto n-alkanoic acid into dimethyl sulfoxide, adding N,N'-carbonyl diimidazole, 1,8-diazabicyclo[5.4.0]undecane-7-ene and choline glycerophosphate, and carrying out a reaction to obtain bis-triphenylmethyl mercapto n-alkanoic acid choline glycerophosphate; 2) dissolving the bis-triphenylmethyl mercapto n-alkanoic acid choline glycerophosphate in dichloromethane, adding trifluoroacetic acid and triethylsilane, and carrying out a reaction to obtain bis-mercapto-alkanoic acid choline glycerophosphate; and 3) dissolving the bis-mercapto-alkanoic acid choline glycerophosphate in dichloromethane, adding n-alkyl dithiopyridine, and carrying out a reaction to obtain the bis-n-alkyl dithio-n-alkanoic acid choline glycerophosphate.
Owner:SOUTHEAST UNIV

Continuous synthesis method of oseltamivir phosphate intermediate

The present invention relates to a continuous synthesis method of an oseltamivir phosphate intermediate, wherein methanesulfonate, triethylsilane, dichloromethane and titanium tetrachloride are subjected to a reaction in a micro channel reactor at a temperature of -10 to -20 DEG C according to a molar ratio of 1:(1-1.5):(25-40):(1-1.5), wherein the residence time of the reaction materials is 10-30min. According to the present invention, the method does not need to carry out the reaction at an ultra-low temperature, and does not require the use of a stainless steel reaction kettle as a reaction device, such that the occurrence of safety accidents is avoided.
Owner:湖南华腾制药有限公司
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