131 results about "Triethylsilane" patented technology

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

The invention relates to a preparation method of canagliflozin, and the preparation method is characterized in that the preparation method comprises the following steps: 1) reacting 2-(4-fluorophenyl)-5-[(5-iodo-2-methylphenyl) methyl ] thiophene with an alkaline reagent and 2,3,4, 6-tetra-O-(trimethylsilyl)- D- glucolactone under a low-temperature condition, and carrying out methylation and deprotection reaction with a methanol solution of methanesulfonic acid to generate an intermediate 1; 2) under a low-temperature condition, reacting the intermediate 1 with triethyl silane and boron trifluoride diethyl etherate, and carrying out post-treatment to obtain an intermediate 2; 3) under a low-temperature condition, reacting the intermediate 2 with an organic base, DMAP and acetic anhydride,and purifying to obtain an intermediate 3; and 4) reacting the intermediate 3 with an alkaline water solution, and purifying after the reaction to obtain the canagliflozin. The method is mild in conditions, safe to operate, simple in post-treatment and high in product purity, no alpha-isomer is detected; the product is safer.