147 results about "Tert-Butanol" patented technology

The invention discloses a preparation method of linolenic acid structural ester with synergistic biological activity, and relates to the technical field of linolenic acid structural ester preparation.The preparation method comprises the steps that specific lipase is prepared through rhizopus wei, and after an SBA-15 molecular sieve is treated, the lipase is fixed to prepare a composite catalyst; the preparation method comprises the following steps: after hydroxyl protection of quercetin, esterifying quercetin with EPA to obtain quercetin-EPA ester; esterifying glycerol and linolenic acid in the presence of a composite catalyst and microwaves, and purifying to obtain an intermediate product; carrying out microwave catalytic ester exchange on the intermediate product and quercetin-EPA ester in tert-butyl alcohol through a composite catalyst to obtain a crude product; and removing impurities from the crude product by a urea adduction method, and carrying out molecular distillation graded purification, column chromatography, deodorization and filtration to obtain a final product. According to the invention, linolenic acid, quercetin and EPA are combined through molecular design to form a compound structure ester with a multi-target effect, and the linolenic acid, quercetin and EPA achieve functional complementation through a synergistic effect, so that the biological activity of the compound structure ester is enhanced.

One form of the present invention provides a double metal cyanide catalyst having excellent catalytic activity and a preparation method thereof. Specifically, the double metal cyanide catalyst according to one form of the present invention is characterized in that it is prepared using a complexing agent comprising tertiary butanol, a linear or cyclic (C2-C12) aliphatic polyol, and a polyalkylene glycol.

The invention relates to the technical field of organic synthesis, in particular to 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine as well as a synthesis method and application of the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine. The synthesis method comprises the following steps: (1) synthesizing 2-chloro-3-fluoro-4-iodine-5-methylpyridine from 2-chloro-3-fluoro-5-methylpyridine and an iodine elementary substance to obtain 2-chloro-3-fluoro-4-iodine-5-methylpyridine; (2) synthesizing 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine, the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride, the tripotassium phosphate and the (2-formyl phenyl) boric acid, and further synthesizing the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine and the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride. And (3) synthesizing the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine by using the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde and sodium tert-butoxide. The 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine compound constructed by the invention can be used for detecting the content of pesticide residue glyphosate.

The invention discloses a preparation method of hydrophobic modified silicon dioxide aerogel with low thermal conductivity. The preparation method comprises the following steps: by taking water glass-tetraethoxysilane as a composite silicon source and formamide-ethylene glycol as a retarder, hydrolyzing and mixing, and then adjusting the pH value to trigger sol-gel reaction to form wet gel; after tert-butyl alcohol aging and solvent replacement, hexamethyldisiloxane and hexamethyldisilazane dual modifiers are used for synchronous hydrophobic modification and sodium removal, and the hydrophobic modified low-thermal-conductivity silicon dioxide aerogel with a porous nanostructure is prepared through freeze drying. The method uses the composite silicon source to cooperate with the gel, so that the raw material cost is reduced; a double-modifier synchronous sodium removal process is green and efficient; the obtained aerogel has low thermal conductivity and excellent hydrophobicity, is suitable for the fields of building thermal insulation, industrial thermal insulation, aerospace and the like, and has the advantages of economy and environmental protection.

This invention discloses a catalyst for the alkylation of tert-butanol with styrene to prepare tert-butylethylbenzene and ethylbenzene, its preparation method, and its application. The catalyst consists of a support and active components loaded on the support. The active components are oxides of rare earth metals and high-valence oxides of transition metals. The support is H-β zeolite. The mass contents of the oxides of rare earth metals and high-valence oxides of transition metals on the support are 3-5% and 2-4%, respectively. This invention makes a breakthrough in the reaction mechanism by loading rare earth metals and transition metals onto a β-molecular sieve and using tert-butanol and styrene as raw materials for alkylation. This avoids the polymerization of styrene (raw material) and the dimerization of isobutylene (intermediate product), reduces the generation of by-products, and makes the catalytic process controllable.

The invention discloses a ruthenium metal complex and a preparation method and application thereof, and belongs to the technical field of organic metal synthesis. The preparation method of the ruthenium metal complex specifically comprises the following steps: (1) under anhydrous and anaerobic conditions, adding ethylene glycol monoethyl ether and RuCl3.H2O into a reaction flask, introducing CO, heating, and reacting; (2) continuously heating, reacting and cooling; and (3) adding 3-chloro-2-methylpropan-1-ene, uniformly mixing, heating, stirring, cooling, adding a potassium tert-butoxide tetrahydrofuran solution, heating until boiling, stirring again, stopping heating, reacting, filtering, cleaning a filter cake with tetrahydrofuran, removing the solvent from the filtrate to obtain a reddish brown oily liquid, and condensing to obtain a Ru (tmm) (CO) 3 product, namely the ruthenium metal complex. The ruthenium metal complex prepared by the method has the advantages of high yield (62.8%), high purity (99.6%), low synthesis cost and simple synthesis steps.

This application relates to the field of organic synthesis technology, specifically disclosing a process for preparing tert-butyl vinyl ether. The raw materials include solid tert-butanol, acetylene, tetrahydrofuran solvent, and potassium hydroxide catalyst, supplemented with auxiliary materials such as type 3A molecular sieves and activated alumina adsorbents. The preparation method involves: after dehydration and purification of the raw materials, the materials are introduced into a reaction vessel; temperature and pressure are controlled, and the reaction endpoint is monitored using an infrared spectrometer; byproducts are quenched and acetylene is recovered; the process involves multi-stage condensation, water washing to remove impurities, distillation separation, and solvent purification and recycling, with simultaneous integration of waste heat recovery and continuous material feeding. The tert-butyl vinyl ether prepared by this process, as an important fine chemical intermediate, can be used in coatings, adhesives, and polymer material modification, possessing advantages such as high purity and good stability. The preparation method achieves efficient utilization of materials and energy through multi-stage synergistic linkage, combining the advantages of green environmental protection, continuous and stable operation, and high resource utilization.

The invention relates to the technical field of synthesis of carbon nitride flame-retardant materials, and particularly discloses a synthesis method of melam, which comprises the following steps: by taking cyanuric chloride as a raw material, carrying out ammoniation and coupling to obtain a bis-triazine intermediate, and carrying out sealed ammoniation on the bis-triazine intermediate by using ammonia water to obtain melam; the optimal potassium tert-butoxide enables the BDCAT to be obtained at the yield of more than 60% in the second-step reaction, the ammonia water ammoniation process used in the third-step reaction is relatively safe, the synthesis method is simple and efficient, and the harsh requirement of a high-temperature and high-pressure method on equipment is avoided.

This invention discloses a bicyclic [2.1.1]hexene compound and its preparation and application. The invention uses bicyclic [1.1.0]butanone and phosphate ester as starting materials, and potassium tert-butoxide tetrahydrofuran solution as base. The reaction is carried out under reflux at 80°C to obtain the bicyclic [2.1.1]hexene compound. The prepared compound has certain transpeptidase inhibitory activity and can effectively inhibit the infection and spread of Staphylococcus aureus.

This invention provides an intelligent control system and method for the production of tert-butane without catalytic reduction, belonging to the field of tert-butane production control. The intelligent control system includes a host computer and sensing and execution mechanisms electrically connected to the host computer. The sensing mechanisms include a TDLAS analyzer installed at the top outlet of the reactive distillation column, NIR analyzers installed at the tert-butanol inlet of the mixing preheater and the side outlet of the reactive distillation column, temperature sensors installed at the top, bottom, and side outlet of the reactive distillation column, flow meters installed at the feed inlet, top outlet, and reflux inlet of the reactive distillation column, and multiple pressure sensors spaced at equal intervals along the height of the reaction section. The execution mechanisms include electrically operated regulating valves installed at the feed inlet and reflux inlet of the reactive distillation column. The control system integrates multiple sensors and execution mechanisms, enabling closed-loop intelligent control of the entire process.

In order to overcome the problems of low initial coulombic efficiency and poor cycle performance caused by insufficient ionic conductivity and large lithium consumption of a solid electrolyte interface film formed by unsaturated carbonate, the invention provides a non-aqueous electrolyte and a secondary battery, the non-aqueous electrolyte comprises a non-aqueous organic solvent, an electrolyte salt and an additive, the additives comprise a first additive, a second additive and a third additive, the first additive comprises a compound as shown in a structural formula 1, and the second additive comprises vinylene carbonate, vinylethylene carbonate, 1, 1, 1, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3 the first additive comprises at least one unsaturated carbonate selected from 1, 2-divinyl ethylidene or 1-methyl-1-vinyl ethylidene carbonate, and the third additive comprises one or two selected from acetone or tert-butyl alcohol; the non-aqueous electrolyte satisfies the following conditions: 10 < = X / Y < = 500, 0.1 < = Z / X < = 30, 10 < = X < = 1000, 1 < = Y < = 5, and 10 < = Z < = 500. The non-aqueous electrolyte provided by the invention can regulate and control the film forming quality of unsaturated carbonate, and effectively improves the first coulombic efficiency and the cycle life of the secondary battery.

This invention relates to the technical field of imiquimod synthesis, specifically to catalysts, methods, and applications for imiquimod synthesis. The invention employs a lipase-immobilized lipase complex carrier to catalyze a transesterification reaction, using vinyl isobutyrate as the acyl donor and tert-butanol as the solvent. The hydroxyl group of 3-(4-amino-1H-imidazo[4,5-C]quinoline-1-yl)-2-methylpropane-1-ol is converted to an isobutyl side chain. Following enzymatic catalysis and pH adjustment, hydrolysis is performed to release the isobutyl group, further generating imiquimod and isobutyric acid. The lipase selectively catalyzes transesterification, avoiding side reactions, and the ester bond is rapidly hydrolyzed to the target product under acidic conditions.

The present invention relates to a process for preparing a double metal cyanide (DMC) catalyst, comprising the reaction of an aqueous solution of a cyanide-free metal salt, an aqueous solution of an alkaline metal cyanide salt, an organic complex ligand and optionally a complex-forming component, wherein the metal cyanide salt is one or more compound(s) and is selected from the group consisting of potassium hexacyanocobaltat(III), potassium hexacyanoferrate(II), potassium hexacyanoferrate(III), calcium hexacyanocobaltate(III) and lithium hexacyanocobaltat(III), where the organic complex ligand is one or more compound(s) and is selected from the group consisting of dimethoxyethane, tert-butanol, 2-methyl-3-buten-2-ol, 2-methyl-3-butyn-2-ol, ethylene glycol mono-tert-butyl ether and 3-methyl-3-oxetanemethanol, and wherein the alkaline metal cyanide salt used has an alkalinity by the titration method disclosed in the Experimental of between 0.700% and 3.000% by weight of sodium hydroxide (NaOH) based on the total weight of the alkaline metal cyanide salt used. The invention further relates to double metal cyanide (DMC) catalysts obtainable by the process according to the invention and to the use of DMC catalysts for preparation of polyoxyalkylene polyols.

The invention discloses a preparation method of 1-amino-2-cyano-1-cyclopentene, which comprises the following steps: 1, preparing a mixed solution, namely mixing a first organic solvent with super alkali in a protective gas atmosphere, heating by adopting a nano infrared energy-saving electric heating coil, stirring, uniformly mixing and dissolving to obtain the mixed solution; the super base is selected from one of potassium tert-butoxide, sodium tert-butoxide, sodium ethoxide, sodium methoxide and sodium hydroxide; 2, cyclization reaction: dropwise adding adiponitrile into the mixed solution, and continuously carrying out infrared heat preservation reaction for 3-8 hours to obtain a reaction solution of 1-amino-2-cyano-1-cyclopentene; 3, cooling crystallization and filtration: cooling the reaction liquid to-10-5 DEG C, standing for crystallization, and carrying out pressure filtration in a protective gas atmosphere to obtain an ACCP crude product and a filtrate; and 4, recrystallizing and refining to obtain a pure product. The method is mild in reaction condition, low in energy consumption, good in product yield and high in product purity, solves the problems of high solvent toxicity, low yield and high environmental protection pressure in the prior art, and is suitable for production of medicine and pesticide intermediates.

The invention belongs to the technical field of potassium tert-butoxide preparation, and particularly discloses a potassium tert-butoxide preparation crystallization tower which comprises a crystallization tower body, the lower portion of one side of the crystallization tower body is connected with an air inlet pipe, the upper portion of one side of the crystallization tower body is connected with a liquid conveying assembly, and the lower portion of the inner wall of the crystallization tower body is connected with a collecting assembly. According to the crystallization tower disclosed by the invention, crystals and a solution falling in the crystallization tower can be collected through the arranged collection assembly, a mother solution can be separated from the crystals, the mother solution can be recycled, waste of a solvent and raw materials is reduced, and the crystallization tower is environment-friendly and energy-saving. Meanwhile, residual crystals and solution on the inner wall of the crystallization tower can be conveniently collected and treated through the cleaning assembly, and the residual crystals and solution on the inner wall of the crystallization tower can be prevented from corroding or abrading equipment, so that the service life of the equipment is prolonged.

This invention relates to a method for preparing a bimetallic cyanide (DMC) catalyst, comprising a reaction of an aqueous solution of a cyanide-free metal salt, an aqueous solution of a basic metal cyanide salt, an organic complexing ligand, and optionally a component forming a complex, wherein the metal cyanide salt is one or more compounds selected from potassium hexacyanocobalt(III), potassium hexacyanoferrate(II), potassium hexacyanoferrate(III), calcium hexacyanocobalt(III), and lithium hexacyanocobalt(III), wherein the organic complexing ligand is one or more compounds selected from dimethoxyethane, tert-butanol, 2-methyl-3-buten-2-ol, 2-methyl-3-butyn-2-ol, ethylene glycol mono-tert-butyl ether, and 3-methyl-3-oxetane-methanol, and wherein the basic metal cyanide salt used has an alkalinity between 0.700 wt% and 3.000 wt% sodium hydroxide (NaOH) based on the total weight of the basic metal cyanide salt used, determined by titration as disclosed in the experimental section. Another subject of the invention includes a bimetallic cyanide catalyst (DMC) obtainable by the method according to the invention, and the use of said DMC catalyst in the preparation of polyoxyethylene polyols.

The present invention discloses a catalyst and a process for preparing anhydrous tert-butanol by isobutene hydration, belonging to the field of industrial catalysis. The preparation of the catalyst comprises the following steps: after polyethylene glycol-polyglycerol-polyethylene glycol triblock polymer, tetraethyl orthosilicate and deionized water are subjected to a first mixing reaction, sodium aluminate and sodium tungstate dihydrate are added for a second mixing reaction to obtain a mixture, and the mixture is successively subjected to calcination and HCl treatment to obtain a pretreated catalyst support. The pretreated catalyst support, a modified ionic liquid and N,N-dimethylformamide are subjected to a third mixing reaction to prepare the catalyst. In the catalyst prepared by the present invention, the lipophilic group adsorbs isobutene, and the hydrophilic group can interact with water molecules. The two effects cooperate with each other to form a microenvironment favorable for the reaction on the surface of the catalyst, thereby improving the conversion rate of isobutene and the selectivity of anhydrous tert-butanol.

The invention relates to the technical field of tert-butyllithium preparation, in particular to a tert-butyllithium preparation method which comprises the following steps: preparing raw materials, dissolving lithium and washing oil, mixing the raw materials to start reaction, dropwise adding a modifier, carrying out heat preservation treatment, cooling, settling and taking clear liquid. According to the method, trace impurities on the surface of lithium are removed in the pretreatment link, the PVP coating can block contact of water, oxygen and lithium in a long-acting mode, lithium is prevented from going bad in the earlier stage of storage and reaction, and meanwhile the compatibility of lithium and organic solvents such as n-pentane is enhanced; the interference of impurities on the reaction can be eliminated in a high-purity state of the chlorinated tert-butane, byproducts such as lithium tert-butoxide are prevented from being generated, the moisture in the system is strictly limited by deep dehydration, a stable anhydrous environment is provided for synthesis of the tert-butyllithium, and the reaction efficiency is guaranteed; the operation of deep dehydration and impurity removal by activated aluminum oxide creates a high-cleanliness solvent system for the reaction, avoids the action of water and polar impurities with tert-butyllithium or reaction intermediates, and prevents product decomposition or impurity generation.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of octadecanedioic acid mono-tert-butyl ester. The method specifically comprises the following steps: reacting dodecanedioic acid, dichloromethane and DMF (Dimethyl Formamide), controlling the temperature, dropwise adding an acylation reagent, and performing reduced pressure concentration after reaction to obtain a compound 1; reacting the compound 1, dimethylbenzene, palladium-carbon and organic alkali, carrying out nitrogen displacement, introducing hydrogen at a controlled temperature, carrying out nitrogen displacement after the reaction, and filtering and concentrating to obtain a compound 2; adding tert-butyl acrylate into an acetic acid aqueous solution, dropwise adding the compound 2, reacting, adjusting the pH value, extracting, filtering and concentrating to obtain a compound 3; adding the compound 3 into dichloromethane, controlling the temperature, adding aluminum trichloride, dropwise adding a reducing agent, reacting, filtering, adjusting the pH value, separating liquid, concentrating and recrystallizing to obtain di-tert-butyl octadecanedioate; and reacting the di-tert-butyl octadecanedioate, lithium hydroxide and tert-butyl alcohol, filtering, adjusting the pH value, extracting, concentrating and recrystallizing to obtain the mono-tert-butyl octadecanedioate. The method is low in production cost and high in safety.

The invention discloses a method for recovering a tert-butyl acetate dealcoholization tower top material. Aiming at the problem that tertiary butanol and diisobutylene in a dealcoholization tower top material are unbalanced in proportion and cannot be directly recycled, the method comprises the following steps: adding a specific entrainer (such as methanol) into the material, and carrying out azeotropic distillation in a tertiary butanol recycling tower by utilizing the characteristic that the entrainer and diisobutylene form a lower-boiling-point azeotrope. An azeotrope of the entrainer and diisobutylene is extracted from the tower top, and an enriched tert-butyl alcohol material which can be directly recycled is obtained from the tower bottom. According to the method, only one rectifying tower unit is needed, the technological process is simple, the azeotrope which is difficult to treat through a traditional method is successfully separated, efficient recycling and cyclic utilization of the tert-butyl alcohol are achieved, it is not needed to purchase the tert-butyl alcohol to adjust the proportion, production raw material consumption and separation energy consumption of the tert-butyl acetate are remarkably reduced, and remarkable energy-saving and consumption-reducing benefits are achieved.

The invention relates to the technical field of organic synthesis, in particular to a synthetic method of 2, 5-dibromobenzoquinone, which takes hydroquinone as an initial raw material and comprises the following two steps: step 1, adding 0.5-2% (based on the mass of hydroquinone) of a phase transfer catalyst (such as tetrabutylammonium bromide) into a glacial acetic acid solvent, reacting with bromine at 10-15 DEG C to generate 2, 5-dibromohydroquinone, and reacting for 2-4 hours at the temperature of 10-15 DEG C to obtain 2, 5-dibromohydroquinone; after the reaction, stably storing an intermediate under the protection of inert gas; 2, oxidizing the 2, 5-dibromohydroquinone into 2, 5-dibromobenzoquinone at the temperature of 45-50 DEG C by taking acetonitrile as a solvent and adopting a tert-butyl hydroperoxide (TBHP)-sodium nitrite composite oxidant (the molar ratio is (10: 1)-(15: 1)); meanwhile, glacial acetic acid and acetonitrile mother liquor generated in the reaction process are subjected to vacuum rectification recovery (the acetonitrile recovery rate is greater than or equal to 90%, and the glacial acetic acid recovery rate is greater than or equal to 88%) for recycling. The invention solves the problems of more brominated byproducts, low oxidation efficiency, solvent waste and unstable intermediate in the prior art.

Multi-carbon compounds such as ethanol, n-butanol, sec-butanol, isobutanol, tert-butanol, fatty (or aliphatic long chain) alcohols, fatty acid methyl esters, 2,3-butanediol and the like, are important industrial commodity chemicals with a variety of applications. The present invention provides metabolically engineered host microorganisms which metabolize methane (CH4) as their sole carbon source to produce multi-carbon compounds for use in fuels (e.g., bio-fuel, bio-diesel) and bio-based chemicals. Furthermore, use of the metabolically engineered host microorganisms of the invention (which utilize methane as the sole carbon source) mitigate current industry practices and methods of producing multi-carbon compounds from petroleum or petroleum-derived feedstocks, and ameliorate much of the ongoing depletion of arable food source “farmland” currently being diverted to grow bio-fuel feedstocks, and as such, improve the environmental footprint of future bio-fuel, bio-diesel and bio-based chemical compositions.

A liquid inlet of an oximation product storage tank is connected with an oximation product liquid inlet pipe, a liquid outlet of the oximation product storage tank is connected with a liquid inlet pipeline of a normal-pressure recovery tower, and a liquid outlet of the normal-pressure recovery tower is connected with a liquid inlet pipeline of a high-pressure recovery tower. A non-condensable gas outlet of the high-pressure recovery tower is connected with a thermal medium inlet pipeline of a reboiler of the normal-pressure recovery tower, a thermal medium outlet of the reboiler is connected with an inlet pipeline of a recovery tank, an outlet of the recovery tank is connected with an inlet pipeline of a high-pressure section condenser, and an outlet of the high-pressure section condenser is connected with an inlet pipeline of a high-pressure section return tank; a gas outlet of the high-pressure section return tank is connected with an inlet pipeline of the ammonia absorption tower, a tertiary butanol outlet of the high-pressure recovery tower is connected with an inlet pipeline of the tertiary butanol storage tank, a liquid outlet of the high-pressure section return tank is connected with an inlet pipeline of the tertiary butanol storage tank, and a liquid outlet of the high-pressure recovery tower is connected with an oximation solution outlet pipe.

This invention discloses a beetle-based nanocellulose aerogel and its preparation method, belonging to the field of oil-water separation materials technology. The invention utilizes a hydrophilic framework formed by chemical crosslinking of lignocellulose nanofibers and polyvinyl alcohol with glutaraldehyde; oleophilic protrusions are formed by coating montmorillonite with graphene; the hydrophilic framework is immersed in a tert-butanol suspension containing the oleophilic protrusions, followed by freeze-drying to obtain the beetle-based nanocellulose aerogel. Due to the heterogeneous structure of the beetle, the hydrophilic framework enables high-speed transport of the aqueous phase, while the oleophilic protrusions efficiently capture and demulsify oil droplets. The synergistic effect of these two mechanisms achieves an ultra-high throughput greater than 10,000 L / m³. ‑2 h ‑1 With a separation efficiency of up to 95%, it effectively alleviates the trade-off between permeation flux and separation efficiency in traditional oil-water separation materials.

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 invention belongs to the field of small molecule synthesis, and particularly relates to a synthesis method of 4-methyl-4, 7-diazaspiro [2.5] octane hydrochloric acid. According to the synthetic route provided by the invention, the target product can be synthesized by only three steps, and the reaction safety and the yield are remarkably improved by optimizing the preparation process of the key intermediate compound 2 and the compound 3 and adopting potassium tert-butoxide and tetraisopropyl titanate to respectively replace dangerous reagents as catalysts. The method is easy and convenient to operate and suitable for industrial production, and an efficient way is provided for synthesis of medical intermediates.

The invention discloses bionic Al2O3 porous ceramic with a bidirectional gradient structure and a preparation method of the bionic Al2O3 porous ceramic, and belongs to the field of ceramic material preparation. Aiming at the problem that a multi-directional gradient structure is difficult to construct by a traditional freezing casting technology, bidirectional gradient regulation and control of a pore structure and components along a freezing direction and a magnetic field direction are realized through a synergistic effect of magnetic field assisted freezing casting and a non-aqueous solvent system. The porous ceramic takes Al2O3 as a matrix, is doped with 3wt.%-9wt.% of Ni powder as a magnetic additive, and takes tert-butyl alcohol (TBA) as a solvent to form bidirectional gradient distribution: the pore diameter and the wall thickness in the freezing direction change in a gradient manner; gradient distribution of a Ni enrichment area (pore orientation parallel magnetic field) and a Ni depletion area (pore orientation parallel freezing direction) is formed in the magnetic field direction. The preparation method comprises the steps of slurry preparation, magnetic field-assisted directional solidification, freeze drying and high-temperature sintering. The method is simple and controllable in process, and is suitable for the fields of biomedical bone repair, environmental filtration, battery energy and the like.

Disclosed in the present invention is a method for preparing a compound of formula 1. The method is shown in the following reaction process. In the method of the present invention, in the presence of a catalyst C1, anhydrous acetaldehyde and diphenyl carbonate are subjected to a one-pot method at a temperature T1 under the condition of an alkali B1 to generate a compound of formula 2, and the compound of formula 2 reacts with tert-butyl hydroperoxide at a temperature T2 by using a catalyst C2 to generate the compound of formula 1. The preparation method of the present invention is simple, has mild reaction conditions and a high reaction yield, and is convenient for industrial production.

The present invention discloses a method for synthesizing tert-butyl (meth)acrylate by using a composite metal oxide catalyst, belonging to the technical field of organic synthesis. In the present invention, a catalyst, an inhibitor, (meth)acrylic acid and isobutene are mixed in a reaction kettle to synthesize tert-butyl (meth)acrylate. The catalyst is a composite oxide WO 3 / Ce x Fe y M z O 2 , wherein M is one or more of Zr, Nb, Sn, Ga, Re, Y, La, Nd, Sm, Er. The inhibitor is a combination of tert-butanol, phenothiazine, p-methoxyphenol, and tert-butylcatechol, and is used in combination with air. The present invention significantly reduces the production cost of tert-butyl acrylate, improves the esterification rate, and effectively prevents the polymerization of raw materials and products during the reaction process. It has the advantages of a simple process route, mild reaction conditions, and easy separation of the catalyst from the raw materials and products.

The invention relates to a cisatracurium besilate process impurity and a synthesis method thereof. The structure of the cisatracurium besilate process impurity is shown as a formula I in the specification. The synthesis method comprises the following steps: 1) adding (1R, 2R)-1, 2, 3, 4-tetrahydro-6, 7-dimethoxy-2-[2-(t-butyloxycarbonyl) ethyl]-2-methyl-1-veratryl isoquinolinium benzene sulfonate into acetonitrile, and adding tert-butyl hydroperoxide to obtain an intermediate A; 2) adding the intermediate A into 70% benzenesulfonic acid, and hydrolyzing to obtain an intermediate B; and 3) adding the intermediate B and (1R, 2R)-1, 2, 3, 4-tetrahydro-6, 7-dimethoxy-2-(9-hydroxy-3-oxo-4-oxynonyl)-2-methyl-1-veratryl isoquinolinium benzene sulfonate into dichloromethane, carrying out reflux, after the reaction is finished, carrying out washing and drying, and carrying out preparation and separation to obtain the cisatracurium besylate process impurity. The impurity can be used as a reference substance for detecting cisatracurium besilate related substances, and is used for controlling the purity of a cisatracurium besilate bulk drug.