24 results about "Tert-butoxy" patented technology

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.

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.

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.

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.

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.

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.

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.

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.

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.

A method for producing a compound represented by formula (2) includes obtaining a compound represented by formula (1) by chemically reacting a compound represented by formula (4) with a compound represented by formula (3), and hydrolyzing the obtained compound represented by formula (1). (In formulae (1) to (4), R1 and R2 are each independently a hydrogen atom, a substituted or unsubstituted C1-6 alkyl group, or the like, R3 is a substituted or unsubstituted C1-6 alkyl group, or the like, and Z is a tert-butoxycarbonyloxy group, a halogen group, or a 1H-imidazole-1-group).

The invention discloses a functionalized ethylene-vinyl alcohol copolymer and a preparation method thereof. The structure of the functionalized ethylene-vinyl alcohol copolymer is shown as a formula 1, wherein M is selected from one of a tert-butoxy group, a tert-pentyloxy group and a copolymer of ethylene and polyvinyl alcohol; x is 0-1, y is 0-1, z is 0-1, and the sum of molar ratios of x, y and z is 1; the weight-average molecular weight of the ethylene-vinyl alcohol copolymer is 20000 to 100000 g / mol; the molecular weight distribution of the ethylene-vinyl alcohol copolymer is 1.0 to 3.0; the ethylene content in the ethylene-vinyl alcohol copolymer is 20 to 50 mol%. The preparation method of the copolymer comprises the following steps: mixing an initiator, peroxide containing acrylic acid, a solvent and vinyl acetate, blowing nitrogen to remove oxygen, introducing ethylene gas, and carrying out pressurized polymerization to obtain the ethylene-vinyl acetate copolymer, and mixing the ethylene-vinyl acetate copolymer, an organic solvent and a catalyst, carrying out alcoholysis reaction, washing with water, filtering and drying to obtain the ethylene-vinyl alcohol copolymer.

The invention provides a preparation method of spirolactone, and relates to the technical field of organic synthesis. The preparation method of spirolactone provided by the invention comprises the following steps: taking 4-androstene-3, 17-diketone as a raw material, carrying out nucleophilic addition reaction on the 4-androstene-3, 17-diketone and an organic zinc reagent 3-tert-butoxy-3-oxypropyl zinc bromide, then carrying out elimination-lactonization under the catalysis of trifluoroacetic acid, and completing lactonization while removing tert-butyl; then sequentially carrying out etherification reaction and oxidative dehydrogenation reaction to obtain canrenone, and finally carrying out addition reaction on canrenone and thioacetic acid to obtain spirolactone. The preparation method provided by the invention provides a novel construction method of 21-carboxylic acid-gamma-lactone, the method is good in specificity, the total mass yield of spirolactone is greater than 92%, and the total mass yield is high; moreover, the HPLC purity of the spirolactone prepared by the preparation method provided by the invention is greater than 99.7%, which is far higher than the purity of the spirolactone prepared by the existing process.

The application discloses an (S)-lenalidomide-5-position derivative, a synthetic method and application thereof, and the application comprises the following steps: removing a tert-butyloxycarbonyl protective group of a compound 1 under acidic conditions to obtain a compound 2; in the presence of an organic amine, the compound 2 is provided with a benzyloxy carbonyl protective group to obtain a compound 3; the compound 3 is subjected to an amination reduction reaction with L-glutamine tert-butyl ester to obtain a compound 4; the compound 4 is subjected to ring closing under acidic conditions to obtain a compound 5; the compound 5 is subjected to a hydrogenation debenzyl-oxy carbonyl reaction with hydrogen under the action of an acid condition and a hydrogenation catalyst to obtain a compound 6; the compound 6 and 7 are subjected to an amination reduction reaction to obtain a compound 8; and the compounds 5, 6 and 8 are (S)-lenalidomide 5-position derivatives. The synthetic method is simple in post-treatment, less in racemization, high in yield, free of toxic pollutants, and safe and environmentally friendly.

The application belongs to the field of fine chemical industry, and discloses a deprotection method of p-tert-butoxyphenethyl methyl ether, which comprises the following steps: heating p-tert-butoxyphenethyl methyl ether under the action of a solid acid catalyst to perform a deprotection reaction, so as to obtain p-(2-methoxy)ethyl phenol; the solid acid catalyst comprises aluminum phosphate and basic metal oxides modified on the aluminum phosphate, and the metal elements contained in the basic metal oxides include one or more of K, Ca, Na, Ba or Mg. The application has the advantages of less three-waste emissions, low operation cost, high production efficiency, and can be used for continuous production of p-(2-methoxy)ethyl phenol, and higher temperature and higher air speed can be adopted.

The present disclosure describes crystalline forms of 2-(tert-butoxy)-4-(3-methyl-3-(5-(methylsulfonyl)isoindolin-2-yl)butyl)phenol fumarate salts and pharmaceutical compositions of same. Also described are methods of using the crystalline forms treating Alzheimer's Disease, Dementia with Lewy Bodies and Dry age-related macular degeneration in a subject in need thereof, comprising administering the crystalline form to the subject. Methods of making the solid forms are also described.

The embodiment of the invention discloses a preparation method of nortropine. The method comprises the following steps: carrying out a demethylation reaction on tropinone and chloroethyl chloroformate in the presence of a solvent, and carrying out vacuum concentration and evaporation to dryness to obtain demethylated tropinone; the preparation method comprises the following steps: carrying out reduction reaction on demethylated tropinone and lithium tri-tert-butoxy aluminum hydride in the presence of a solvent to obtain the nortropine alcohol. According to the method, a novel reducing agent lithium tri-tert-butoxy aluminum hydride is adopted, the reducing agent is safe and insensitive to air and water, aftertreatment is simple, and potential safety hazards are avoided from the source; the use of dangerous Raney nickel is avoided, and an autoclave is not needed, so that the production capacity is greatly improved; the reaction is carried out under a low-temperature condition, the energy consumption is low, the production cost can be effectively reduced, the reaction condition is mild, the operation is safe, simple and convenient, and large-scale industrial production is facilitated.

The invention discloses an electrolyte, a preparation method and a sodium ion battery using the electrolyte. The electrolyte comprises an organic solvent, a functional cosolvent, a functional additive and conductive sodium salt, the organic solvent is composed of 1, 2-diethoxyethane and 1, 2-di-tert-butoxy ethane; the functional cosolvent is adiponitrile; the functional additive is p-nitroanisole; the conductive sodium salt is composed of sodium bis (fluorosulfonyl) imide and sodium hexafluorophosphate or sodium difluoro (oxalato) borate. The preparation method comprises the following steps: pretreating raw materials (dehydration and vacuum drying), proportionally mixing the organic solvent and the cosolvent in an inert atmosphere, adding the conductive sodium salt, stirring and dissolving, adding the functional additive, uniformly stirring, curing and filtering to obtain the electrolyte. Through unique collaborative design of non-fluorinated components, stable operation of the electrolyte under ultrahigh voltage and efficient regulation and control of an interface are realized.

Disclosed is a catalyst combination comprising at least two catalysts useful to aid in curing a moisture curable silicone polymer composition, which may comprise: a first catalyst comprising a titanium (IV) diisopropoxide bis (acetylacetonate); and a second catalyst comprising tert-butoxy titanium (IV); wherein the described catalyst combination is useful in a moisture-curable silicone polymer reaction, optionally wherein the curable material comprises a moisture-curable organosiloxane, a moisture-curable silane-modified polymer, or a combination thereof, and preferably the catalyst combination, and the composition comprising the catalyst combination is free of tin.

The invention relates to the technical field of medicine analysis and detection, in particular to a method for detecting related substances of (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido] tert-butyl propionate hydrochloride. The detection method comprises the following steps: detecting by adopting a high performance liquid chromatography; wherein the chromatographic conditions are as follows: a chromatographic column is an octadecyl silane bonded silica gel chromatographic column; an aqueous solution of alkali is used as a mobile phase A, acetonitrile and / or methanol is used as a mobile phase B, and gradient elution is carried out. The detection method disclosed by the invention can be used for accurately, stably, reliably and sensitively analyzing and detecting impurities existing in a process route based on (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido] tert-butyl propionate hydrochloride, and has very important significance on quality research and control of the INR101 injection.

The present application relates to the technical field of pharmaceutical analysis and detection, and particularly relates to a detection method of (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido]propionic acid tert-butyl ester hydrochloride related substances. The detection method comprises: using high performance liquid chromatography for detection; wherein, the chromatographic conditions comprise: the chromatographic column is an octadecylsilane bonded silica gel chromatographic column; using an aqueous alkali solution as mobile phase A, and using acetonitrile and / or methanol as mobile phase B for gradient elution. The detection method can accurately, stably and reliably analyze and detect the impurities existing in the process route based on (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido]propionic acid tert-butyl ester hydrochloride, and has very important significance for the quality research and control of INR101 injection.

The present disclosure describes crystalline forms of 2-(tert-butoxy)-4-(3-methyl-3-(5-(methylsulfonyl)isoindolin-2-yl)butyl)phenol fumarate salts and pharmaceutical compositions of same. Also described are methods of using the crystalline forms treating Alzheimer's Disease, Dementia with Lewy Bodies and Dry age-related macular degeneration in a subject in need thereof, comprising administering the crystalline form to the subject. Methods of making the solid forms are also described.

The invention relates to the technical field of polymer synthesis, in particular to poly (4-tert-butoxystyrene) resin as well as a preparation method and application thereof. The preparation method comprises the following steps: respectively and independently introducing a 4-tert-butoxystyrene monomer, an initiator and a protective agent into a microreactor, and carrying out anionic polymerization reaction to obtain a reaction solution; and sequentially carrying out quenching, precipitation and solid-liquid separation on the obtained reaction liquid to obtain the poly (4-tert-butoxystyrene) resin. According to the preparation method disclosed by the invention, the protective agent is introduced and is synergistically matched with the initiator, so that the defects of wide molecular weight distribution, more side reactions and high metal impurity content of the poly (4-tert-butoxystyrene) resin caused by incompatibility of an organic lithium initiator and an ether bond-containing monomer in the prior art are overcome. The preparation method is simple and convenient to operate, stable and reliable in product quality and easy to realize industrial large-scale production.

The invention discloses a synthetic method and application of 4-tert-butoxystyrene, in an organic solvent system, p-hydroxystyrene and di-tert-butyl dicarbonate are reacted under the catalytic action of perchlorate to obtain 4-tert-butoxystyrene, the molar ratio of p-hydroxystyrene to perchlorate is (5-15): 1, the molar ratio of p-hydroxystyrene to perchlorate is (5-15): 1, and the molar ratio of p-hydroxystyrene to perchlorate is (5-15): 1. The molar ratio of the p-hydroxystyrene to the di-tert-butyl dicarbonate ester is 1: (1.8-2.2); the reaction time is 4-8 hours; the present invention; the preparation process is simple and easy to control, the total production time is shortened, the production cost is reduced, the purity of the obtained product is up to 99.5 or above, the impurity total amount is low, the variety is few, the turbidity and moisture of the product are low, the requirements of electronic-grade raw materials are completely met, and the prepared product meets the requirement for producing photoresist matrix resin.

The application discloses a kind of 1-allyl hydrazine carboxylic acid tert-butyl ester, its preparation method and purposes.The application uses tert-butoxy formyl hydrazine as raw material, after imino protection, N-allylation intermediate is obtained, and after deimino protection, the target product is obtained.The synthesis method is simple in operation, mild in condition, high in yield and good in repeatability, without using toxic hydrazine reagent, without column separation operation.The preparation method provided by the application is simple in process, low in cost, mild in reaction condition and easy to control, safe and reliable in production process, and suitable for industrialization.