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61 results about "Tert-butoxy" patented technology

Preparation method of p-tert-butoxystyrene

The invention relates to the technical field of organic synthesis, in particular to a preparation method of p-tert-butoxystyrene. According to the preparation method provided by the invention, the p-tert-butoxystyrene is prepared by utilizing the continuous flow microreactor, the operation is simple and safe, the efficiency is high, the reaction time is short, the temperature is low, expensive reagents are not used, the amplification effect does not exist, the prepared p-tert-butoxystyrene product is high in yield and purity and stable in quality, and the method is suitable for large-scale production and has wide application prospects. The production cost can be greatly reduced, and the production safety is improved.
Owner:SHANGHAI BAYI SPACE ADVANCED MATERIAL CO LTD

Separation and detection method of enantiomer in (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido] tert-butyl propionate hydrochloride

PendingCN120490350AComponent separationPropizochlorPropanoic acid
The invention belongs to the field of detection and analysis, and relates to a method for separating and detecting enantiomers in (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido] tert-butyl propionate hydrochloride. According to the method, HPLC is adopted for separation and detection, a polysaccharide derivative chiral chromatographic column is selected as a chromatographic column, a mobile phase A is a weak base aqueous solution, and a mobile phase B is acetonitrile and / or methanol. The method is strong in specificity, high in separation degree, high in accuracy, stable, reliable and high in sensitivity, and a simple, accurate, rapid and reliable detection method is provided for control of impurities in a starting material of (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido] tert-butyl propionate hydrochloride.
Owner:YUNNUO PHARMACEUTICAL (TIANJIN) CO LTD +1

Small molecule boron-10 carrying agent, preparation method and application

The invention relates to a small molecular boron-10 carrying agent, a preparation method and application. The structural formula of the small molecule boron-10 carrying agent is shown as a formula (I). The invention also provides a preparation method of the small molecular boron-10 carrying agent, which comprises the following steps: carrying out condensation connection on a phenylboronic acid derivative and N-(2-aminoethyl) maleimide hydrochloride, and covalently coupling a boron drug to obtain a first intermediate; n < 2 >-(((9H-fluorene-9-yl) methoxy) carbonyl)-N < 6 >-(tert-butoxycarbonyl)-L-lysine, N-(2-aminoethyl) maleimide hydrochloride and a phenylboronic acid derivative are subjected to condensation connection, and a second intermediate is obtained; carrying out esterification connection on a selenium-containing compound and a DNA repair inhibiting compound to obtain a third intermediate; and carrying out condensation connection on the second intermediate and the third intermediate, and connecting the first intermediate to obtain the small molecule boron-10 carrying agent. The invention solves the problems of limited treatment effect and difficulty in inhibiting DNA damage repair in the existing BNCT. # imgabs0 # (I)
Owner:DONGGUAN PEOPLES HOSPITAL

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

Preparation method of Fmoc-Lys (Ivdde)-OH

The invention provides a preparation method of Fmoc-Lys (Ivdde)-OH, which comprises the following steps: reacting dimedone with isovaleric acid under the action of a condensing agent to generate an intermediate compound, then reacting with N-alpha-tert-butoxycarbonyl-L-lysine under the action of organic alkali to obtain an intermediate, then reacting with acid to obtain an intermediate, and finally, separating and purifying the intermediate to obtain the Fmoc-Lys (Ivdde)-OH. Finally, under the action of inorganic alkali, the Fmoc-Lys (Ivdde)-OH reacts with fluorenylmethoxycarbonyl succinimide, and Fmoc-Lys (Ivdde)-OH is obtained. According to the method provided by the invention, the diketone is taken as a starting raw material, Fmoc-Lys (Ivdde)-OH is synthesized through four steps of reaction including two-step condensation reaction, Boc removal reaction and Fmoc feeding reaction, the process is simplified, the operation is simple, the reaction condition is mild, the industrial production difficulty is reduced, expensive raw materials are not involved, the production cost is favorably controlled, and the obtained product is high in purity and high in yield.
Owner:四川什邡市三高生化实业有限公司

Preparation method of dipeptide-2

The invention provides a preparation method of dipeptide-2, which comprises the following steps: dissolving (S)-2-((tert-butoxy) amino)-3-methylbutyric acid, N-hydroxysuccinimide and dicyclohexylcarbodiimide in an organic solvent I under the protection of inert atmosphere, reacting at 10-30 DEG C for 8-30 hours, filtering, and concentrating filtrate under reduced pressure until the filtrate is dry to obtain an intermediate 1; controlling the temperature to be-5 DEG C to 5 DEG C, mixing the intermediate 1, L-tryptophan and an organic solvent II, adding an alkaline reagent, reacting at 20-40 DEG C for 12-30 hours after adding, then adding water and ethyl acetate for extraction, retaining an ethyl acetate phase, and concentrating under reduced pressure to be dry to obtain an intermediate 2; dissolving the intermediate 2 in an organic solvent III, adding an acidic reagent I, reacting at 10-30 DEG C for 2-30 hours after the addition is completed, concentrating to dryness, then dissolving in an acidic reagent II, adjusting the pH value to 6-7, finally adding a dipeptide-2 seed crystal, crystallizing, filtering and drying to obtain the dipeptide-2. The purity of the dipeptide-2 prepared by the method is greater than 99%, and the yield is high.
Owner:PANZHIHUA UNIV

Method for preparing side chain intermediates of telpotitide

The invention provides a method for preparing a telpotide side chain intermediate, which comprises the following steps: by taking 20-(tert-butoxy)-20-oxo-eicosanoic acid as a starting material, forming an active anhydride intermediate by using alkyl chloroformate, adding a strong alkali solution of 1-tert-butyl L-glutamic acid, reacting, adjusting the acid, extracting a product by using ethyl acetate, combining organic phases, concentrating and drying to obtain M2; taking M2 as a raw material, forming an active anhydride intermediate by using alkyl chloroformate, adding a strong alkali solution of AEEA-AEA, reacting, adjusting the acid, extracting a product by using ethyl acetate, combining organic phases, concentrating, and drying to obtain M4; and finally, taking M4 as a raw material, forming an active anhydride intermediate by using alkyl chloroformate, adding a strong alkali solution of Fmoc-lysine, reacting, adjusting the acid, extracting a product by using ethyl acetate, combining organic phases, concentrating, purifying, and drying to obtain the product. According to the method, amido bonds are formed in one pot, so that the purification process of the intermediate is reduced, the experimental steps are optimized, and the experimental cost is reduced.
Owner:PANZHIHUA UNIV

Core-shell polyacrylamide nano flocculant as well as preparation method and application thereof

The invention relates to a core-shell polyacrylamide nano flocculant as well as a preparation method and application thereof, the flocculant is of a core-shell structure, the shell is a water-soluble polyacrylamide polymer, and the core is cross-linked poly (p-hydroxystyrene); the preparation method comprises the following steps: preparing a poly (p-tert-butoxystyrene-b-polyacrylate) block polymer or a poly (4-acetoxystyrene-b-polyacrylate) block polymer; carrying out hydrolysis and self-assembly on poly (p-tert-butoxystyrene) or poly (4-acetoxystyrene) on the block polymer at the same time in the presence of a trifluoroacetic acid hydrolysis reagent by utilizing a modification induced self-assembly process, and carrying out in-situ crosslinking on poly (p-hydroxystyrene) obtained by hydrolysis by using formaldehyde; and in the presence of a 1, 5, 7-triazabicyclo [4.4. 0] decene-5-ene catalyst, modifying the polyacrylate block by using an amination reagent to prepare the flocculant. Compared with the prior art, the flocculant provided by the invention has the advantages of controllable morphology, stable cross-linkable property and the like.
Owner:FUDAN UNIVERSITY

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

A high styrene solution styrene butadiene rubber, and a preparation method and application thereof

PendingCN122325672APolymer scienceNew energy
The application provides a high-styrene solution polymerized styrene-butadiene rubber and a preparation method and application thereof, and the preparation method comprises the following steps: mixing styrene, butadiene, an initiator, a structure regulator and a non-polar solvent, and performing a polymerization reaction to obtain solution polymerized styrene-butadiene rubber; wherein the structure regulator comprises at least two of t-butoxy sodium, t-amyl oxy sodium, 2,3-dimethyl-3-pentanol sodium and ethylene glycol disodium, and a crown ether. By using the composite structure regulator, the application can prepare a random high-styrene content solution polymerized styrene-butadiene rubber, and the rubber almost does not contain styrene blocks, and the content of vinyl in the rubber can be adjusted by the addition amount of the structure regulator. Therefore, the solution polymerized styrene-butadiene rubber prepared by the application has good strength and hardness due to the high styrene content, and the random microstructure reduces the glass transition temperature and heat build-up of the raw rubber, and is suitable for the manufacturing of high-performance tires such as new energy vehicle tires.
Owner:PETROCHINA CO LTD

A method for synthesizing a styrene-based photoresist resin

This invention discloses a method for synthesizing styrene-based photoresist resin, comprising the following steps: adding styrene and p-tert-butoxystyrene to a DES solvent, ultrasonically dispersing the mixture, and then rapidly adding an initiator under an air atmosphere to obtain a styrene-p-tert-butoxystyrene copolymer, i.e., a styrene-based photoresist resin, via anionic polymerization. The preparation method of this invention is simple and the process is easy to control. Using DES as the polymerization solvent allows the reaction to proceed efficiently under ambient air atmosphere. Furthermore, the hydrogen bond network in DES can form a specific interaction with the oxygen atom in the p-tert-butoxy group, resulting in a significant stabilizing effect on this acid-sensitive protecting group and effectively suppressing the removal of the protecting group and the resulting side reactions during anionic polymerization.
Owner:HEBEI UNIV OF SCI & TECH

Preparation method of N-hydroxyurea compound

The invention discloses a preparation method of an N-hydroxyurea compound, which specifically comprises the following steps: step 1, sequentially carrying out Lossen rearrangement and nucleophilic reaction under the action of alkali by taking Boc NHOH as shown in a formula 1 as an initial reactant, SO2F2 gas as an acylating agent and an amine compound RR 'NH as a nucleophilic reagent to obtain a tert-butoxyurea compound as shown in a formula 2; and 2, removing the tert-butoxy group from the tert-butoxyurea compound to obtain the N-hydroxyurea compound as shown in a formula 3. The innovation point of the invention is that commercialized easily available gas sulfonyl fluoride promotes Lossen rearrangement of tert-butylhydroxylamine to generate a key intermediate tert-butoxy isocyanate, the key intermediate tert-butoxy isocyanate and a substrate amine compound are subjected to a one-pot reaction to obtain the N-hydroxyurea compound, the reaction conditions are simple, the operation is convenient, the compatibility of substrate functional groups is strong, and the application prospect is good.
Owner:ZHEJIANG UNIV OF TECH

Synthesizer for preparing modified pigment red 254 from di-tert-butyl dicarbonate

The utility model discloses a synthesis device for preparing modified pigment red 254 from di-tert-butyl dicarbonate. A discharge hole in the bottom of a first reaction kettle is connected with a feed hole of a second reaction kettle through a first transfer pump; a feeding hole of the second reaction kettle is connected with a tetrahydrofuran storage tank through a second transfer pump; a discharge hole in the bottom of the acyl chloride preparation tank is connected with a constant-pressure dropping device through a third transfer pump, and the constant-pressure dropping device is connected with a feed hole of the second reaction kettle; a gas inlet of the second reaction kettle is connected with a carbon dioxide gas cylinder through an anti-suck-back device; a bottom discharge port of the second reaction kettle is connected with a feed port of the third reaction kettle through a fourth transfer pump; a top gas outlet of the second reaction kettle is connected with the first washing type tail gas treatment equipment. According to the device, tert-butoxycarbonyl is introduced to imino groups of the pigment for modification, so that an intermolecular hydrogen bond net is destroyed, and insoluble pigment is changed into soluble modified pigment.
Owner:INNER MONGOLIA XISHANGXI NEW MATERIAL TECH CO LTD

Composition for forming charge transport thin films

A composition for forming a charge-transporting thin film containing a charge-transporting precursor having a 9-tert-butoxycarbonylcarbazole structure within the molecule and an organic solvent provides a thin film exhibiting good charge-transporting properties even when sintered at low temperatures. Furthermore, the aforementioned charge-transporting precursor can be used to prepare the composition using a low-polarity solvent that causes less damage to substrates and components made of organic compounds compared to highly polar amide solvents.
Owner:NISSAN CHEM CORP

Synthesis method of 1H-indazole-7-tert-butyl formate

The invention discloses a synthesis method of 1H-indazole-7-tert-butyl formate, and belongs to the technical field of organic synthesis. The synthesis method of the 1H-indazole-7-tert-butyl formate comprises the following steps: dissolving 7-carboxyl-1H-indazole in an organic solvent I, then adding 1, 1-di-tert-butoxy-N, N-dimethyl methylamine, heating, and carrying out a stirring reaction to obtain a reaction solution; and performing post-treatment. According to the synthesis method, one-step conversion of indazole carboxylic acid into indazole tert-butyl formate is achieved, reaction conditions are mild, aftertreatment and purification are simple, cost is low, and manufacturability amplification can be achieved.
Owner:上海毕得医药科技股份有限公司

Modified perfluoropolyether electrolyte with wide electrochemical window and lithium ion battery

The invention relates to a modified perfluoropolyether electrolyte with a wide electrochemical window and a lithium ion battery. The modified perfluoropolyether electrolyte is characterized by comprising modified perfluoropolyether and a lithium salt, wherein the structural general formula of the modified perfluoropolyether is A-R-Rf-R-B, in the formula, Rf is a perfluoropolyether chain segment, and perfluoropolyether comprises one or more of K type perfluoropolyether, D type perfluoropolyether, Y type perfluoropolyether or Z type perfluoropolyether; r is a non-fluoroether chain segment, and the non-fluoroether chain segment comprises one or more of a methyleneoxy group, an ethyleneoxy group, a propoxy group, an isopropoxy group, a n-butoxy group, a sec-butoxy group, an isobutoxy group, a tert-butoxy group or a pentyloxy group; a and B are independently selected from one of hydroxyl, methoxyl or benzoate. Compared with the prior art, the modified perfluoropolyether electrolyte is prepared by mixing the modified perfluoropolyether and the lithium salt, and the electrochemical stability window of the modified perfluoropolyether electrolyte is remarkably improved.
Owner:PETROCHINA SHANGHAI ADVANCED MATERIALS RESEARCH INSTITUTE CO LTD +1

Temperature-responsive cellulose-based hydrogel and preparation method thereof

PendingCN120118339ACelluloseTert-butoxy
The invention discloses a temperature-responsive cellulose-based hydrogel and a preparation method thereof, and relates to a cellulose-based hydrogel and a preparation method thereof. The invention aims to solve the problems that the LCST can be obviously improved after a hydrophilic substance is added into the existing PNIPAM gel, and the success rate of preparing the gel with high transparency at low temperature is low. The temperature response cellulose-based hydrogel is prepared from deionized water, N-isopropylacrylamide, 2-hydroxy-3-tert-butoxy propyl hydroxyethyl cellulose, ammonium persulfate, N-N methylene bisacrylamide and sodium hydrogen sulfite, and the temperature response cellulose-based hydrogel is prepared from the deionized water, the N-isopropylacrylamide, the 2-hydroxy-3-tert-butoxy propyl hydroxyethyl cellulose, the ammonium persulfate, the N-N methylene bisacrylamide and the sodium hydrogen sulfite. The method comprises the following steps: 1, preparing a 2-hydroxy-3-tert-butoxy propyl hydroxyethyl cellulose crude product; 2, dialyzing, freezing and drying; (3) weighing; 4, mixing; and 5, carrying out low-temperature reaction. The invention is used for the temperature-responsive cellulose-based hydrogel and the preparation thereof.
Owner:NORTHEAST FORESTRY UNIV

Preparation method and application of lithium tri-tert-butoxy aluminum hydride-tetrahydrofuran solution

The invention relates to the technical field of chemical engineering, in particular to a preparation method and application of a lithium aluminum tri-tert-butoxyhydride-tetrahydrofuran solution. Industrial-grade tert-butyl alcohol is purified through molecular distillation to obtain purified tert-butyl alcohol, the purified tert-butyl alcohol and anhydrous tetrahydrofuran are mixed to prepare a tert-butyl alcohol-tetrahydrofuran solution, and then the tert-butyl alcohol-tetrahydrofuran solution is prepared into the lithium aluminum tri-tert-butoxyhydride-tetrahydrofuran solution. The method comprises the following steps: mixing a lithium aluminum hydride solid with anhydrous tetrahydrofuran, and stirring to obtain a lithium aluminum hydride-tetrahydrofuran suspension; conveying the tert-butyl alcohol-tetrahydrofuran solution and the lithium aluminum hydride-tetrahydrofuran suspension into a microchannel reactor with ultrasonic waves through a double-plunger metering pump, and reacting to obtain a product solution; and stirring the product solution, adding 2, 6-butylated hydroxytoluene, and filtering to obtain a lithium aluminum tri-tert-butoxy hydride-tetrahydrofuran solution. The continuous flow reaction is assisted by ultrasonic waves, high-efficiency and high-selectivity preparation is realized, and a stable solution product is obtained.
Owner:GANSU JUNMAO NEW MATERIAL TECH CO LTD

A process for the preparation of norpinozol

ActiveCN121378243BSolventChloroethyl chloroformate
The embodiment of the present application discloses a preparation method of nor-tropine alcohol. The method comprises the following steps: performing demethylation reaction on tropinone and chloroethyl chloroformate in the presence of a solvent, performing vacuum concentration and evaporation, and obtaining demethyltropinone; performing reduction reaction on the demethyltropinone and lithium tri-t-butoxyaluminum hydride in the presence of a solvent, and obtaining the nor-tropine alcohol. The present application adopts a new type of reducing agent lithium tri-t-butoxyaluminum hydride, which is safe, not sensitive to air and water, and simple in post-treatment, thus avoiding safety hazards from the source. The present application avoids the use of dangerous Raney nickel and does not need to use an autoclave, so that the production capacity is greatly improved. The present application performs the reaction under low-temperature conditions, is low in energy consumption, can effectively reduce production cost, and is moderate in reaction conditions, safe and simple in operation, and is conducive to large-scale industrial production.
Owner:BEIJING MEDIKING BIOPHARM

Process for preparing 2-( tert-butoxy)-4-(3-methyl-3-(5-methylsulfonyl)isoindolin-2-YL)butyl)phenol

The present invention provides processes for the preparation 2-(t-butoxy)-4-(3-methyl-3-(5-methylsulfonyl)isoindolin-2-yl)butyl)phenol The disclosed processes overcome drawbacks of prior art methods by providing safer, more efficient synthetic routes with improved yields and reduced impurity levels. A key improvement includes a novel photochemical bromination process using continuous flow technology. The invention also encompasses novel intermediates including compounds of Formula 12 and 13. The processes eliminate the use of hazardous reagents, reduce reaction times, and provide better control over product purity, making them suitable for large-scale pharmaceutical manufacturing.
Owner:COGNITION THERAPEUTICS INC

Continuous synthesis method of p-tert-butoxychlorobenzene

The invention discloses a continuous synthesis method of p-tert-butoxychlorobenzene, and belongs to the technical field of organic synthesis. The method comprises the following steps: continuously pumping a parachlorophenol solution and an isobutene solution into a tower reactor for reaction, and continuously feeding a reaction solution into an extraction tower for separation and purification. According to the invention, the tower reactor is combined with continuous extraction, so that the whole process from reaction to post-treatment is continuous, and the production efficiency is greatly improved; according to the method, efficient reaction can be realized under mild conditions, the process control is stable, side reaction is effectively inhibited, and the product yield is high; meanwhile, equipment is safe and reliable, the comprehensive production cost is remarkably reduced, and the method is suitable for industrial large-scale application.
Owner:SHANDONG HANXING PHARM TECH CO LTD +1

Nanoscale targeted health intervention nutritional ingredient embedding method

The invention relates to a nanoscale targeted health intervention nutritional ingredient embedding method, and belongs to the technical field of ingredient embedding. The specific embedding method comprises the following steps: preparing 1-[(tert-butoxy) methyl]-4-iodobenzene by utilizing iodobenzene methanol or tert-butyldimethylsilyl chloride solution; adding selenium powder, a first catalyst and alkali, and reacting to obtain 1-[(t-butoxy) methyl]-4-({4-[(t-butoxy) methyl] phenyl} disilyl) benzene; trifluoroacetic acid is added for a reaction, and bis (4, 1-hydroxy benzyl) diselenide is obtained; dissolving the mixed solution, EGCG and a second catalyst in an organic solvent to obtain a mixed solution containing EGCG; dropwise adding an oxalyl chloride solution into the mixed solution containing EGCG for reaction to obtain a SeOE polymer; the preparation method comprises the following steps: emulsifying and homogenizing a SeOE polymer solution and a polyvinyl alcohol solution, centrifuging and freeze-drying to obtain the SeOE polymer nanoparticles. According to the invention, by introducing an ROS sensitive chemical part, the ROS removal capability of the targeted delivery polymer and the oxidation stability of EGCG are improved.
Owner:ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES +1

Curable polyorganosiloxane composition and cured product thereof, protective agent or adhesive and electrical / electronic device

Provided is a curable polyorganosiloxane composition which has excellent storage stability in the form of a single liquid, has good curability and adhesiveness even at relatively low temperatures, and has an appropriate usable time. Specifically, provided is a curable polyorganosiloxane composition which has excellent curability even at a temperature of 80 DEG C or less and which has excellent adhesion to resins such as polyesters and polyphenylene sulfide. A one-pack type curable polyorganosiloxane composition comprising the following components (A) to (E): (A) a polyorganosiloxane having at least two alkenyl groups in one molecule; (B) a polyorganosiloxane having at least two silicon atoms bonded to hydrogen atoms in one molecule; (C) a hydrosilylation reaction catalyst; (D) a condensation reaction catalyst selected from the group consisting of titanium tetra-tert-butoxy, titanium bis (isopropoxy) bis (ethyl acetoacetate), and a chelate aluminum complex, or a condensation reaction product thereof; and (E) a curing inhibitor. The silicone rubber composition having a JIS A hardness of 5 or more is provided by curing. The composition may optionally contain a large amount of (H) an inorganic filler or the like.
Owner:DOW TORAY CO LTD +1

Method for continuously preparing (2R, 4S)-5-(biphenyl-4-yl)-4-[(tert-butoxycarbonyl) amino]-2-methylpentanoic acid

The invention belongs to the technical field of organic synthesis, and particularly relates to a method for continuously preparing (2R, 4S)-5-(biphenyl-4-yl)-4-[(tert-butoxycarbonyl) amino]-2-methylpentanoic acid, which comprises the following steps: dissolving and mixing, S2, carrying out hydrogenation reaction, S3, quenching and concentrating, S4, crystallizing and filtering, and S5, continuously drying: carrying out vacuum drying on a filter cake to obtain a target product (2R, 4S)-5-(biphenyl-4-yl)-4-[(tert-butoxycarbonyl) amino]-2-methylpentanoic acid. According to the present invention, the continuous hydrogenation reaction, the crystallization and the drying process are performed on the (4S, 4S)-5-(biphenyl-4-yl)-4-[(t-butoxycarbonyl) amino]-2-methylpentanoic acid, such that the batch interval time of the traditional intermittent production is avoided, the productivity per unit time is significantly improved, the method is suitable for industrial amplification, and the reaction time is shortened due to the use of the fixed bed reactor or the micro-channel mixer.
Owner:SUZHOU NO 4 PHARMA FACTORY

Phenylalanine-tryptophan dipeptide skeleton mesoporous silicon material as well as preparation method and application thereof

The invention provides a phenylalanine-tryptophan dipeptide skeleton mesoporous silicon material and a preparation method and application thereof.The preparation method comprises the steps that phenylalanine and tryptophan serve as raw materials to synthesize N-tert-butoxycarbonyl phenylalanyl tryptophan, the N-tert-butoxycarbonyl phenylalanyl tryptophan reacts with N-tert-butoxycarbonyl ethanediamine, then the N-tert-butoxycarbonyl phenylalanyl tryptophan reacts with N-tert-butoxycarbonyl N-tert-butoxycarbonyl is removed to obtain phenylalanyl tryptophan-ethanediamine hydrochloride, and then the phenylalanyl tryptophan-ethanediamine hydrochloride reacts with 3-isocyanate propyl triethoxy silane to obtain a phenylalanyl tryptophan dipeptide organic silicon precursor; mixing with tetraethyl orthosilicate according to a ratio, slowly dropwise adding into an acidic mixed solution of a template agent, deionized water and sodium chloride, carrying out water bath overnight, and carrying out high-temperature crystallization, suction filtration, water washing and drying at room temperature, so as to obtain the high-performance molecular sieve. And removing the template agent by using a mixed solvent of absolute ethyl alcohol and hydrochloric acid through a Soxhlet extractor, and drying at room temperature to obtain phenylalanine-tryptophan dipeptide skeleton mesoporous silicon materials with different proportions. The dipeptide skeleton meso-porous silicon material obtained by the method can effectively adsorb chloramphenicol, the adsorption capacity can reach 90mg / g, in addition, the influence of the external environment on the chloramphenicol is reduced, and the stability of the chloramphenicol is improved.
Owner:NANJING TECH UNIV

Preparation method of high-purity amino acid benzyl ester hydrochloride

The invention relates to the technical field of medicine synthesis, in particular to a preparation method of high-purity amino acid benzyl ester hydrochloride. The high-purity amino acid benzyl ester hydrochloride is prepared by carrying out tert-butoxycarbonyl protection reaction, coupling reaction, tert-butoxycarbonyl deprotection reaction and recrystallization on amino acid. The preparation method provided by the invention does not need to use toxic organic solvent benzene, benzyl alcohol and a catalyst, so that the synthesis cost is saved, a large amount of wastewater is not generated in the synthesis process, the operation flow is simplified, and the synthesis route is safer and more environment-friendly. The method effectively solves the problems that the existing method for synthesizing the amino acid benzyl ester hydrochloride needs to use a toxic solvent, a large amount of wastewater is generated in the synthesis process, impurities are easy to introduce, and the product purity is low, and provides a new thought for synthesis of the high-purity amino acid benzyl ester hydrochloride.
Owner:HEFEI NUOXIN BIOTECHNOLOGY CO LTD

A kind of water-repellent polyester fiber and preparation method thereof

The invention relates to a water-repellent polyester fiber and a preparation method thereof. First, a terminal hydroxyl hyperbranched polyester and an asymmetric alcohol hydroxyl mono-terminated polydimethylsiloxane are subjected to a dehydration reaction to obtain a terminal siloxane hyperbranched polyester, and then polyethylene terephthalate I, a terminal siloxane hyperbranched polyester and a dimethylvinylsiloxy cage-shaped polysilsesquioxane are melt-blended to prepare a water-repellent polyester functional masterbatch, and then polyethylene terephthalate II and the water-repellent polyester functional masterbatch are blended and melt-spun, and finally the surface of the fiber obtained by melt spinning is coated with tri-tert-butoxyvinylsilane, and then a grafting reaction is induced by ultraviolet radiation to obtain the water-repellent polyester fiber; the number average molecular weights of polyethylene terephthalate I and polyethylene terephthalate II are both within the range of 20000-30000 g / mol; and the contact angle of the water-repellent polyester fiber is greater than 145°. The method of the invention is simple, and the obtained product has good mechanical properties and water repellency.
Owner:JIANGSU HENGLI CHEM FIBER

Triazine ring-containing polymer, method for producing triazine ring-containing polymer, and non-photosensitive liquid composition

The invention relates to a triazine ring-containing polymer, a method for producing the triazine ring-containing polymer, and a non-photosensitive liquid composition. The present invention addresses the problem of providing: a triazine ring-containing polymer capable of providing a molded article having a high refractive index and excellent light resistance or heat resistance; a method for producing the triazine ring-containing polymer; and a non-photosensitive liquid composition containing the triazine ring-containing polymer. [Solution] A liquid crystal composition containing a compound having a tert-butoxycarbonyloxy group, a triazine ring-containing polymer having a structural unit having a structure in which an aromatic group of a tert-butoxycarbonylamino group, a hydroxyl group protected by an acetal protecting group, or a carboxyl group protected by an acid-dissociable group is bonded to a triazine ring via a specific linking group, a polymer containing a triazine ring contains a structural unit that includes a structure in which an aromatic group is bonded to the triazine ring via a specific linking group and that is different from the structural unit, or a terminal group having a specific structure is bonded, or the weight-average molecular weight of the polymer containing the triazine ring is 4,000-20,000 (inclusive).
Owner:TOKYO OHKA KOGYO CO LTD