96 results about "Reaction step" patented technology

The invention discloses a synthetic method of a water soluble ultraviolet light absorber BP-9. The method mainly comprises the following process steps: (1) carrying out methylation on the main raw materials of 2, 2', 4, 4'-tetrahydroxyl benzophenone, a transition metal salt catalyst and a mixed solvent which is prepared from dichloroethane and anhydrous ethanol in equal parts by weight to obtain 2, 2'-dihydroxyl-4, 4'-dimethoxyl benzophenone; (2) carrying out sulfonation reaction on the main raw materials of methylate, sulfamic acid and C1-C3 halohydrocarbon to obtain 2, 2'-dihydroxyl-4, 4'-dimethoxyl benzophenone-5, 5'-disulfonic acid; and (3) carrying out neutral reaction on the main raw materials of sulfonated product, inorganic base and ethanol water to finally obtain the BP-9 product. The synthetic method disclosed by the invention is few in reaction step, low in cost, high in product purity and stable in quality, and raw materials are easily available.

The present application relates to a kind of phenol and methanol directly prepared (methyl) anisole mode, the method includes the following steps: under the action of composite catalyst, phenol and methanol are catalytically generated methyl anisole, the composite catalyst is Ho / β molecular sieve catalyst and Ti / UiO-66 with mass ratio Ho / β:Ti / UiO-66 0.3-0.6:1 Mixed composite catalyst.The process reaction step is simple, and synthesis is realized in one step, and the total selectivity of methyl anisole is as high as 76% or more, and can be continuously and stably operated for 3000h.

The application discloses a preparation method of a key intermediate of dapagliflozin, and belongs to the technical field of preparation of medical intermediates. The preparation method of the key intermediate of dapagliflozin comprises the following steps: 1, 1-ethoxy-4-methylbenzene is prepared by using p-cresol, sodium hydroxide and diethyl sulfate; 2, (4-ethoxybenzyl) phenyl sulfide is prepared by using 1-ethoxy-4-methylbenzene, thiophenol, a palladium catalyst, an alkali and an oxidant; 3, 1-benzyl-4-ethoxybenzene is prepared by using (4-ethoxybenzyl) phenyl sulfide under a hydrogen atmosphere; 4, 4-ethoxy-2'-chlorobenzhydrol is prepared by carrying out chlorination reaction on 1-benzyl-4-ethoxybenzene; and 5, 5-bromo-2-chloro-4'-ethoxybenzhydrol is prepared by carrying out bromination reaction on 4-ethoxy-2'-chlorobenzhydrol. The yield and purity of 5-bromo-2-chloro-4'-ethoxybenzhydrol prepared by the method are higher, the process is safer, and the production cost is reduced.

The present application relates to a kind of from androsta 1, 4-diene-3, 17-dione starting synthesis of estren and the method of a kind of compound thereof.Especially, the present application provides a kind of preparation method of estren shown in formula I, comprising the following steps: in inert solvent, androsta-1, 4-diene-3, 17-dione (II) with reagent R4VX carries out demethylation aromatization reaction step directly to obtain estren (I);Wherein, the definition of reaction substrate, reagent and reaction condition is as claimed in claim or specification.The method is simple in operation, and good in selectivity, and product purity is high, suitable for industrial production.

To perform measurement based on polarization anisotropy in which a reaction between a target substance and a luminescent reagent is performed within a short period of time, and in which high-sensitivity measurement can be performed, provided is an analysis method including measuring a value (R) for polarization anisotropy through use of a luminescent reagent that reacts with a target substance, to thereby determine at least any one of the presence or absence of the target substance and a concentration of the target substance, the analysis method including: a reaction step of mixing a sample containing the target substance with the luminescent reagent, and subjecting the mixture to a reaction to obtain a reaction liquid; a dilution step of diluting the reaction liquid to obtain a diluted liquid; and a measurement step of measuring the R of the diluted liquid, the luminescent reagent including luminescent particles.

The application relates to a method for synthesizing lithium sulfide based on micro-channel continuous flow and multi-stage gradient temperature control, and belongs to the technical field of lithium-sulfur batteries. The method solves the technical problems of low mass transfer efficiency, insufficient temperature control precision, poor product stability and the like in the existing lithium sulfide synthesis process. The method comprises the following steps: S1, pretreating raw materials; S2, configuring lithium hydroxide organic suspension by using the pretreated lithium hydroxide and anhydrous N-methyl pyrrolidone; S3, constructing a micro-channel reaction system and performing pretreatment; S4, mixing and reacting lithium hydroxide organic suspension and pretreated hydrogen sulfide in the micro-channel reactor; S5, performing solid-liquid separation on the liquid after the reaction in step S4; and S6, performing solvent recovery and hydrogen sulfide recycling treatment. Compared with the prior art, the application has the advantages of high temperature control precision, excellent stability, energy saving and carbon reduction, and economic and environmental benefits.

The present invention relates to a method for producing nitrile by controlling the input pressure of a spraying liquid and a production apparatus. The method can atomize the spraying liquid, increase the contact area with ammonia, and improve the mass transfer efficiency. The method for producing nitrile includes a step of producing a reaction product containing nitrile by subjecting a hydrocarbon raw material to an ammoxidation reaction (referred to as a reaction step), and a step of spraying a spraying liquid to the reaction product by a spraying device to cool the reaction product (referred to as a cooling step), wherein the spraying device includes a spraying liquid inlet, a first spraying pipe in fluid communication with the spraying liquid inlet, a plurality of second spraying pipes in fluid communication with the first spraying pipe and extending to both sides of the first spraying pipe perpendicularly thereto, a plurality of third spraying pipes in fluid communication with the second spraying pipes and extending to both sides of the second spraying pipes perpendicularly thereto, and a nozzle at the end of the third spraying pipes and in fluid communication therewith, and wherein the input pressure of the spraying liquid of the spraying liquid inlet is controlled to 0.06-1.00 MPaG in the cooling step.

The application discloses a preparation method of a trans-7H-pyrrolo[2,3-d]pyrimidine compound, and the full name of the trans-7H-pyrrolo[2,3-d]pyrimidine compound is trans-N-methyl-4-(methyl-7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)cyclohexylmethanesulfonamide maleate, which is prepared from trans-4-[(tert-butoxycarbonyl)amino]cyclohexane carboxylic acid and 4-chloro-7H-pyrrolo[2,3-d]pyrimidine as starting materials through reduction, chlorination, substitution, oxidation, methylation, condensation and salt formation reactions. The preparation method has the advantages of few reaction steps, simple operation, low production cost, high production efficiency, high yield, high product purity and suitability for scale-up production.

Disclosed is a preparation method for cannflavin compounds. The preparation method has the advantages of cheap and easily available raw materials, few reaction steps, short production period, simple operation, etc. The method comprises: firstly, condensing 4′-hydroxy-3′-methoxyacetophenone and diethyl carbonate (DEC) under an alkaline condition to obtain 4′-hydroxy-3′-methoxybenzoyl acetate; reacting 1,3,5-trihydroxybenzene with bromo-isoamylene under an alkaline condition to obtain 2-isopentenyl-1,3,5-trihydroxybenzene; and finally, condensing 4′-hydroxy-3′-methoxybenzoyl acetate and 2-isopentenyl-1,3,5-trihydroxybenzene at a high temperature to produce cannflavin B and / or isocannflavin B, and then subjecting same to separation and purification to obtain pure cannflavin B and pure isocannflavin B.

This invention relates to the field of pharmaceutical impurity preparation technology, and discloses a method for synthesizing apixaban genotoxic impurity I. The steps include: S1. performing an addition reaction of compound II in an alkaline system to generate compound III; S2. subjecting the product of S1 to elimination and isomerization reactions under heating, separating the reaction product to obtain apixaban genotoxic impurity I. The synthesis method of this invention has high safety, low raw material cost, and can achieve a one-pot reaction while ensuring yield and product purity (no product separation and purification is required between each reaction step; only one separation and purification is needed after obtaining the final product).

This invention belongs to the technical field of lithium-ion battery cathode materials, specifically relating to a lithium iron phosphate composite material, its preparation method, and its application. The invention first modifies the surface of lithium iron phosphate powder using a carboxymethyl cellulose-based mixed material in an organic solvent system. Then, using the surface-treated lithium iron phosphate powder as a matrix, stearate-based surfactants as dispersants, and carboxylic acids such as formic acid as catalysts, an electrode material modified with a PEDOT / PSS conductive polymer is generated in situ. This method has advantages such as simple reaction steps, easy temperature control, and small and uniform particle size of the resulting powder. Furthermore, the conductivity of the modified lithium iron phosphate electrode material is significantly improved.

This invention discloses a method for synthesizing a tenapano hydrochloride intermediate. The synthesis method includes the following steps: (1) condensing the compound 3-bromophenylacetaldehyde and the compound N-methyl-(2,4-dichlorophenyl)methylamine under dehydration conditions to obtain an enamine intermediate; (2) subjecting the enamine intermediate to an intramolecular cyclization reaction in the presence of an acid catalyst to obtain the tenapano hydrochloride intermediate 4-(3-bromophenyl)-6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinoline. The synthetic route provided by this invention requires only two steps to construct the key framework, and has the advantages of short reaction steps, high overall yield, and no need to use highly toxic liquid bromine. This process has high atom economy, reduces the emission of waste gas, wastewater, and solid waste, and is suitable for large-scale industrial production under mild conditions.

This invention provides a manufacturing method that can produce high-purity quaternary ammonium salts with high yield. [Solution] A reaction step to obtain an ammonium halide compound by reacting a tertiary amine with a (substituted) benzyl halide compound, and the halide ions contained in the ammonium halide compound obtained in the reaction step are (C6F5)4B - SbF6 - PF6 - (CF3CF2)3PF3 - (C6F5)4Ga - A method for producing quaternary ammonium salts is used, which includes a salt exchange step in which the salt is exchanged in a solvent with at least one ion selected from the group consisting of trifluoromethanesulfonate anion and p-toluenesulfonate anion, and the entire process from the reaction step to the salt exchange step is carried out using a continuous production facility.

The utility model provides a light excitation chemiluminescence immunoassay reagent disc, which comprises a disc body and a reaction hole unit arranged on the disc body, and the reaction hole unit comprises a pre-reaction hole, a main reaction hole and a signal amplification hole which are sequentially connected in series to form a three-stage reaction channel; independent micro heating films are respectively integrated at the bottoms of the pre-reaction hole, the main reaction hole and the signal amplification hole; connecting runners are arranged between the pre-reaction hole and the main reaction hole as well as between the main reaction hole and the signal amplification hole, and fluid flow is controlled through centrifugal force or capillary force; a micro-column array or a micro-cavity array is arranged in the pre-reaction hole, and the surface of the micro-column array is modified with a biomolecule capture layer; a micro-nano composite structure is arranged in the main reaction hole, and enzyme or probe molecules are immobilized on the surface of the micro-nano composite structure. According to the utility model, the technical problems of insufficient reaction steps and low temperature control precision of the reagent disc in the prior art can be effectively solved.

The application provides a preparation method of silicon nitride, comprising the following steps: direct reaction: passing silane gas and ammonia gas into a reactor, controlling the temperature of the reactor to be 600-900 DEG C, and making the silane gas and the ammonia gas react to form amorphous silicon nitride; phase transformation: controlling the reactor to be heated to 1000-1300 DEG C, and passing silicon powder into the reactor, so that the amorphous silicon nitride obtained in the direct reaction step is transformed into alpha-phase silicon nitride, and the silicon powder reacts with the ammonia gas to obtain alpha-phase silicon nitride. According to the application, the silane gas and the ammonia gas are made to react at low temperature to form amorphous silicon nitride, the energy consumption and the production cost of the reaction are reduced, then the temperature is increased and the silicon powder is passed in, the amorphous silicon nitride is transformed into alpha-phase silicon nitride, and the silicon powder acts as a diluent for the nitriding reaction, so that the quality and the purity of the alpha-phase silicon nitride powder obtained finally are high.

This invention discloses a method and apparatus for preparing aromatics from methanol. The method includes: sequentially performing a hydrocarbonation reaction and an aromatization reaction on methanol under the action of a hydrocarbonation catalyst to obtain an aromatization product; performing preliminary separation on the aromatization product to obtain a light component, mixed aromatics, and water, with the light component returned to the aromatization reaction step; separating the mixed aromatics to obtain light aromatics and heavy aromatics; and performing a cracking reaction on the heavy aromatics under the action of a cracking catalyst, with the cracking product returned to the preliminary separation step. The process flow, catalyst selection, and three-stage reaction conditions of this application for preparing aromatics from methanol achieve gradient separation and directional conversion of the reaction products, effectively suppressing side reactions and improving the purity and yield of the target product.

This invention provides a method for preparing quinolone compounds, belonging to the field of pharmaceutical intermediate synthesis technology. The invention involves mixing a phenolic compound, a fluorosulfonating reagent, an organic base, and an organic solvent to perform a fluorosulfonation reaction, yielding a fluorosulfonated product. The fluorosulfonated product, a borate ester compound, a transition metal catalyst, a ligand, an inorganic base, and a solvent are then mixed and coupled to obtain the quinolone compound. The purpose of this invention is to address the problems existing in current synthetic methods for C7 carbon-carbon bond-substituted quinolone compounds, such as long reaction steps, low yields, and numerous hazardous processes. It provides a new synthetic method for quinolone compounds, requiring inexpensive and readily available chemical reagents, featuring a short process, high yield, and avoiding the use of hydrogen or diazonium salts, making it suitable for both rapid laboratory synthesis and industrial production.

This invention discloses a method for preparing highly substituted polyanionic cellulose, comprising the following steps: 1) alkalizing a system consisting of refined cotton, organic solvent, and alkaline solution by introducing excess organic amine gas and stirring; 2) after alkalization in step (1), heating and depressurizing to remove the organic amine gas, and then adding an etherifying agent to the reaction system for reaction; 3) after the reaction in step (2), the product is neutralized with acetic acid, filtered, washed with excess 90% ethanol, filtered again, dried, and pulverized to obtain highly substituted polyanionic cellulose. This invention promotes the degree of alkalization of cellulose and increases the degree of subsequent etherification reaction. The degree of substitution of the polyanionic cellulose prepared by this invention can reach over 1.40, which is higher than the degree of substitution of products prepared by ordinary solvent methods, and has high application value.

The application discloses a mild synthesis method of a selenium-containing urea-based benzimidazole derivative, and the method is characterized by that 1,2-diisocyanobenzene derivative, secondary amine and elemental selenium (Se powder) are used as reaction raw materials, one-pot cyclization reaction is carried out in the presence of a solvent and an additive at room temperature in an air atmosphere, and after reaction, the selenium-containing urea-based benzimidazole derivative is prepared through separation and purification, wherein R 1 is H, 4-Me, 4-CO2Me, 4,5-di-Cl, 4,5-di-Me, R 2 is C6H5, 4-MeC6H4, 4-NH2C6H4, 4-CF3C6H4, 1-naphthyl, 2-pyridyl, i-Pr, R 3 is Me, i-Pr, Bn. The synthesis method disclosed by the application is characterized by simple reaction steps, excellent yield of target products and wide application range of substrates.

This plasmalogen detection method comprises: a sample preparation step for mixing a Schiff's reagent and a specimen containing a plasmalogen to obtain a sample; a reaction step for reacting the plasmalogen in the sample with the Schiff's reagent; and a contact step for bringing at least some of the sample reacted in the reaction step into contact with a stationary phase containing a silica gel.

The application discloses a residual oil alkali metal treatment-catalytic cracking combined processing method, which comprises the following steps: (1) mixing residual oil raw materials and alkali metals into a reactor to perform reaction; (2) performing solid-liquid separation on the material after the reaction in step (1) to obtain a solid-phase product and generated oil; and (3) feeding the generated oil obtained in step (2) into a catalytic cracking device, and performing fractionation on the material after the reaction to obtain dry gas, liquefied gas, catalytic cracking gasoline, catalytic cracking light diesel oil, catalytic cracking heavy distillate oil and coke. The method can produce high-quality low-sulfur gasoline fraction, has a long running cycle, does not need high-temperature and high-pressure conditions and has low hydrogen consumption, thereby effectively improving fuel quality, reducing device running cost, realizing energy saving and consumption reduction.

The application belongs to the field of chemical synthesis, and particularly relates to a preparation method of high-selectivity ethylene glycol monoethyl ether, and reaction steps comprise: under the protection of inert gas, etherification reaction of ethylene glycol and ethanol is generated to form ethylene glycol monoethyl ether in the presence of heteropolyacid salt / molecular sieve supported catalyst. The supported catalyst used by the application has a special structure, and has very high selectivity to the generation of ethylene glycol monoethyl ether. In addition, the application still has high conversion rate and selectivity under large-scale production (ten kilogram level), and the reaction condition is more moderate compared with the prior art, and is suitable for industrial production.

This invention discloses a core-shell catalyst for the dehydrogenation of methanol to polyoxymethylene dimethyl ether (POMDE), its preparation, and its application. The catalyst comprises an acidic molecular sieve, a metal active component, and aluminum-containing mesoporous silica. The acidic molecular sieve serves as the core structure, with the metal active component coating the surface of the acidic molecular sieve to form a first coating layer, and the aluminum-containing mesoporous silica coating the surface of the metal active component to form a second coating layer. The prepared core-shell catalyst uses the middle acidic molecular sieve and the outermost aluminum-containing mesoporous silica as acidic sites, and the middle metal active component as a dehydrogenation site. By integrating these two reaction sites, a bifunctional catalyst is constructed, achieving in-situ coupling of the two-step reactions of methanol dehydrogenation to formaldehyde and methanol-formaldehyde condensation to POMDE. This not only simplifies the reaction steps but also improves the selectivity of the reaction.

This invention relates to the field of lithium battery electrolyte technology, specifically a method for synthesizing tripropynyl phosphate, comprising the following steps: 1) In a dry reaction vessel, an organic solvent is added, and phosphorus oxychloride is dissolved in the organic solvent, and stored under an inert atmosphere at low temperature; 2) A mixture of propynyl alcohol and triethylamine is slowly added dropwise, and the reaction is continuously stirred while maintaining a low temperature; 3) The mixture is slowly added dropwise, and the reaction is stirred after the temperature is raised to room temperature; 4) The mixture is slowly added to the reaction vessel, and the reaction is stirred after the temperature is raised to room temperature; 5) The triethylamine hydrochloride is removed by filtration, and the filtrate is distilled under reduced pressure to obtain a crude product, which is then purified by reduced pressure distillation or column chromatography. This invention effectively solves the problems of violent exothermic reactions, numerous side reactions, harsh reaction conditions, and difficulties in post-processing and purification of the product in existing synthesis methods by rationally designing reaction steps and precisely controlling reaction conditions and molar ratios.

This invention discloses a highly efficient oxygen removal reagent and its application in the deoxygenation reconstruction of carbon resource molecular skeletons, comprising a pivot reagent, a phosphine reagent, an azo reagent, a reducing agent, an acid reagent, a base reagent, a photosensitizer, and an organic solvent; wherein, X in the pivot reagent includes a hydrazine group or a sulfone group; PG is a protecting group; LG is a leaving group; by using natural oxygen-containing functional groups such as alcohols, aldehydes, and ketones as direct coupling precursors, an integrated in-situ activation-deoxygenation coupling process is achieved, significantly reducing reaction steps.

The application discloses a method for preparing reduced graphene oxide by a gas-solid phase one-step method and belongs to the technical field of graphene preparation. The method comprises the following steps: step 1, a certain proportion of combustible gas and air is introduced into a combustion furnace to make the combustible gas and air have an incomplete combustion reaction, and high-temperature gas containing carbon monoxide and hydrogen is generated; step 2, the high-temperature gas of the combustion furnace is used for preparing graphene oxide powder and thermal reduction reaction of graphite intercalation compounds; and step 3, the reactants in step 2 are cooled, then gas-solid separation is carried out, and the obtained solid is graphene powder. The combustible gas is convenient and cheap, a high-temperature and reduction gas atmosphere is created, the graphite intercalation compound continuously completes the powder preparation and the reduction of graphene oxide in a closed environment, the production of the reduced graphene oxide has ideal production efficiency and product yield, and the production cost is relatively low.

The application provides a cobalt acetate crystal preparation method based on waste cobalt residue and the cobalt acetate crystal. The preparation method comprises the following steps: S1, hydrogen reduction is performed on the waste cobalt residue to obtain a reduction product; S2, the reduction product is added into an inorganic acid solution, and a cobalt salt product is obtained through first stirring; S3, the cobalt salt product is added into an inorganic alkali solution, and a precipitation product and a residual liquid are obtained through second stirring; S4, the precipitation product is mixed with acetic acid, and the cobalt acetate crystal is obtained after reaction; the waste cobalt residue is a cobalt-containing waste catalyst generated in the oxidation reaction of trimethylphenol to trimethylbenzoquinone by using a supported cobalt catalyst. Through the design and optimization of the reduction, dissolution, precipitation and reaction steps of the waste cobalt residue, the waste cobalt residue is effectively utilized, the recycling of resources is realized, the cobalt acetate crystal prepared has high purity, low impurity content and good application performance.

The application discloses a particle size control method of titanium dioxide, which comprises the following steps: adding sodium chloride into a mixed flow field of titanium tetrachloride and oxygen, wherein the sodium chloride reacts with the titanium tetrachloride and the oxygen to generate an intermediate and chlorine; with the reaction proceeding, the oxygen is gradually reduced, the chlorine is increased, and the intermediate reacts with the chlorine to generate sodium chloride and titanium dioxide again. The scheme provided by the application introduces an additive into a reaction system of titanium tetrachloride and oxygen, so that a rapid and severe exothermic reaction originally completed in one step is decomposed into two or more reaction step sequences. In this way, the huge reaction heat concentrated in an instant is dispersed into multiple stages and released gradually, so that the sharp accumulation of heat is fundamentally avoided, and the safe and stable control of the reaction exothermic rate is realized.

The application discloses a kind of silica-based Janus particles and its preparation method and application, its preparation method includes the following steps: the molar ratio of 1:0.007~0.014 of silicate and alkoxysilane is dissolved in solvent, after stirring, a certain amount of weak alkaline solution is added, after 20~30 ℃ reaction 6~12 h, after centrifugation, dry and obtain silica-based Janus particles.The method needs lower temperature for reaction, mild condition, reaction step is less, and the Janus particles prepared are uniform spherical shape, the surface of the ball has obvious different morphology, one side is smooth and the other side is rough, the smooth surface has hydrophilicity and the rough surface has lipophilicity, which can be applied to stable emulsion, catalyst loading, drug controlled release and other fields.

This invention discloses a method for the etherification of 5-cyanodiol hydrochloride to citalopram bromate using a dehydration membrane. The method includes: adding 5-cyanodiol hydrochloride, toluene, and a strong acid resin catalyst to a round-bottom reaction flask equipped with a magnetic stirrer; placing a water separation membrane in the reaction flask; maintaining a high vacuum on the permeate side of the water separation membrane; and then heating the reaction on a magnetically stirred heater. In the toluene system, the water separation membrane removes the water generated in situ through vapor permeation, driving the reaction forward, breaking the thermodynamic equilibrium constraint, improving product yield and purity, and achieving coupling of reaction and separation. This invention uses a strong acid resin catalyst coupled with a water separation membrane, resulting in a simple reaction procedure and favorable reaction conditions; the catalyst is safe and stable, with a low risk factor, is a green catalyst, can be recycled, and is easily separated from the reaction liquid; the water separation membrane removes water in situ through vapor permeation, improving raw material conversion rate and product purity.