305results about How to "High reaction yield" patented technology

The invention discloses a p-methyl benzyl chloride production process and a production system thereof, p-xylene side chains and chlorine are subjected to a gas phase substitution reaction under micro negative pressure and visible light catalysis to generate crude methyl benzyl chloride and hydrogen chloride, and 99.0% methyl benzyl chloride, a small amount of benzyl dichloride and 31% hydrochloric acid are respectively generated through rectification and absorption; the device consists of four working sections of chlorination, rectification, hydrochloric acid absorption and distillation. According to the method, the defects in the prior art are overcome, on one hand, chlorine is introduced, and an aromatic ring chlorination reaction is carried out under visible light catalysis; on one hand, a supported catalyst filler is arranged at the bottom of a chlorination tower, and a zeolite molecular sieve modified by long-chain alkylsilane and supported by metal salt is used as a catalyst to catalyze chloromethylation reaction, on the other hand, the hydrophobicity of the modified catalyst is obviously enhanced, and meanwhile, the density of acidic sites is not reduced; the contact opportunity of the catalyst and a reaction substrate is greatly increased, and the catalytic efficiency of the catalyst is improved.

The invention discloses a method for synthesizing pyroxasulfone, which comprises the following steps: by taking a raw material A and air as raw materials, carrying out oxidation reaction under the catalysis of a Fe (III) catalyst to obtain pyroxasulfone. The method has the advantages of mild reaction conditions, high yield, less three wastes, avoidance of hydrogen peroxide use and storage reactions, low cost and suitableness for industrial production.

The present invention provides a preparation method of 4,6-dihydroxypyrimidine, and the preparation method comprises the following steps: adding a mixed solution of malonate and formamide to an alkali metal alcoholate / solvent containing a catalyst, and then keeping the mixture warm for reaction after the addition is completed. After the reaction is completed, the solvent is evaporated to dryness, and after being dissolved in water, the mixture is acidified to a pH of 2-3, filtered, washed with water, and dried to obtain 4,6-dihydroxypyrimidine. The present invention utilizes a catalyst to catalyze the reaction, thereby improving the reaction yield, having a high atomic economy, and reducing the amount of raw materials used, reducing the generation of saline wastewater, and alleviating environmental pressure.

The invention belongs to the field of fluorine-containing fine organic chemical synthesis, and particularly relates to a method for continuously and cleanly producing perfluoroolefin epoxide by using hydrogen peroxide. The invention relates to a method for continuously and cleanly producing perfluoroolefin epoxide by using hydrogen peroxide, which comprises the following steps of: reacting perfluoro-2-methyl-2-pentene serving as a raw material in the presence of a polar solvent and hydrogen peroxide serving as an oxidant under the action of a catalyst to obtain perfluoro-2-methyl-2, 3-epoxypentane. The method has the beneficial effects that the micro-reactor is used, and the oxidizing agent, the catalyst, the cocatalyst and the polar solvent are continuously introduced into the pipeline of the micro-reactor, so that the synthesis from the hexafluoropropylene dimer to the epoxy compound is completed in a short time.

The invention provides a preparation method and application of magnesium L-threonate, and belongs to the technical field of medicines. The preparation method comprises the following steps: dissolving L-ascorbic acid in water, adding magnesium hydroxide and alkaline magnesium carbonate, stirring, dropwise adding hydrogen peroxide, heating, stirring and reacting, filtering a product, purifying and concentrating by temperature-sensitive molecularly imprinted hydrogel while the product is hot, adding an ethanol water solution into a concentrated solution, standing, crystallizing, filtering, washing and drying to obtain the magnesium L-threonate. And cooling the temperature-sensitive molecularly imprinted hydrogel after adsorption to room temperature, washing and repeatedly using the temperature-sensitive molecularly imprinted hydrogel. The magnesium L-threonate is simple in preparation method, high in purity and high in yield, meanwhile, the slow-release magnesium L-threonate is prepared, and the magnesium L-threonate is low in toxicity, good in biocompatibility, large in drug loading capacity, low in economic cost and good in drug effect and has wide application prospects in preparation of anti-depression drugs.

The invention discloses a synthesis method of a 2 '-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3'-indoline] derivative, and belongs to the technical field of organic synthesis.The 2 '-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3'-indoline] derivative is obtained by synthesizing 2 '-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3'-indoline] in the presence of visible light, a photocatalyst and alkali. CF3Br and a 3-(3-hydroxypropyl) indole derivative are subjected to a free radical tandem cyclization reaction in an organic solvent to prepare the 3-(3-hydroxypropyl) indole derivative. According to the 2 '-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3'-indoline] derivative and the preparation method thereof, CF3Br is used as a trifluoromethyl source under photocatalysis for the first time, trifluoromethyl is directly introduced into an indoline ring of 4, 5-dihydro-spiro [furan-2, 3 '-indoline], the 2'-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3 '-indoline] derivative is obtained, and the compound has good activity and selectivity on cancer cells such as Huh-7, A549 and A549 / DDP.

The utility model discloses equipment for producing high-purity methyl ethyl ether, which relates to the field of synthesis of chemical compounds and comprises a reaction device, a heating component, a cold bath tank, a crude product receiving tank, a heavy component removal tower, a light component removal tower, a first reboiler, a second reboiler, a first condenser, a second condenser, a recovery tank, a product receiving tank and a controller, raw materials including sodium methoxide and halogenated ethane directly react under the anhydrous condition, a catalyst is not needed, crude methyl ethyl ether is produced, then the crude methyl ethyl ether enters a heavy component removal tower, crude methyl ethyl ether gas with heavy components removed enters a light component removal tower from the top of the light component removal tower after being detected to be qualified through a first online analysis and detection component, light component removal rectification is conducted, and methyl ethyl ether is obtained. Gas-phase impurities at the top of the light component removal tower are analyzed through the second online analysis and detection part, when the gas-phase impurities are detected to be qualified, the methyl ethyl ether product enters the product receiving tank, and then the high-purity methyl ethyl ether product is produced through continuous rectification, so that the product purity is high, the reaction temperature is low, the energy consumption is reduced, the reaction yield is high, and the production cost is low.

The invention discloses a method for preparing tetrakis hydroxymethyl phosphonium sulfate by using high-concentration hydride, and belongs to the technical field of preparation of tetrakis hydroxymethyl phosphonium sulfate. The method for preparing tetrakis hydroxymethyl phosphonium sulfate by using the high-concentration hydride comprises the following steps: step 1, adding concentrated sulfuric acid and formaldehyde into a reaction kettle, uniformly stirring and mixing, then adding an organic catalyst and a modified surfactant, and continuously stirring to completely and uniformly mix reactants to obtain a mixed solution; 2, hydride is introduced into a reaction kettle through a pipeline and reacts with the mixed solution, a heating reaction is conducted, after the reaction is finished, the pipeline is closed, and a reaction solution is obtained; and 3, carrying out vacuum concentration treatment on the reaction liquid, and recrystallizing to obtain tetrakis hydroxymethyl phosphonium sulfate. The tetrakis hydroxymethyl phosphonium sulfate prepared by the method has excellent yield and purity.

The invention discloses a preparation method of 1alpha-hydroxyl dinorhydrin, the structural formula of the 1alpha-hydroxyl dinorhydrin is shown as a formula (1), the method comprises the following steps: by taking dinorhydrin shown as a formula (2) as a raw material, preparing the 1alpha-hydroxyl dinorhydrin through five steps of acylation, bromination, debromination, epoxidation / hydrolysis and ring opening, and the reaction formula is as follows: # imgabs0 #. All reactions are carried out under normal pressure, reagents with high toxicity are not used in the reaction process, the reaction yield is high, the total yield of the five-step reaction can reach 48.46%, and the method is suitable for industrial production.

The invention discloses a preparation method of a 1-(aryl sulfuryl) bicyclo [1.1. 0] butane compound, which comprises the following steps: reacting a compound 1 serving as a raw material with trisubstituted propane and an alkaline reagent in a reaction solvent in an air-isolated environment under the action of an organic catalyst and a metal catalyst at the temperature of-78 to 200 DEG C for 1 to 48 hours to obtain the 1-(aryl sulfuryl) bicyclo [1.1. 0] butane compound. And obtaining a compound 2 after complete reaction. The key raw materials in the synthesis route are cheap and easy to obtain, the reaction conditions are mild, the operation is convenient, the process safety is high, the selectivity is high, the yield is high, the product purity is high, the production cost is greatly reduced, and the production requirement of the product at the ton level or above can be fully met.

The invention discloses a preparation method of carbonyl fluoride, which comprises the following steps: with hexafluoropropylene and oxygen as raw materials, introducing gas into a reactor filled with a catalyst for reaction at high temperature; the catalyst is one of palladium oxide, ruthenium oxide, platinum oxide and molybdenum oxide. According to the scheme, the cost is low, the raw material utilization rate is high, and compared with other carbonyl fluoride synthesis methods, the reaction does not involve phosgene, fluorine and other dangerous chemicals, and reaction by-products are few. In addition, according to the method, the toxicity of raw materials is small, hexafluoropropylene can be completely reacted under the condition of excessive oxygen, the reaction process is environment-friendly and simple, and basically no three wastes are generated. According to the method, hexafluoropropylene and oxygen are adopted as raw materials which are common chemical raw materials and are cheap and easy to obtain, and the method is simple in reaction process, mild in reaction, easy to operate and suitable for industrial production.

The invention discloses a method for green and safe synthesis of epsilon-caprolactone from cyclohexanone, and belongs to the technical field of heterocyclic compound and organic chemical raw material manufacturing, and the method comprises the following steps: oxidizing and converting cyclohexanone into a mixture aqueous solution of epsilon-caprolactone, 6-hydroxyhexanoic acid and 6-hydroxyhexanoic acid linear oligomers / oligomers, removing peroxides in the mixture aqueous solution, and obtaining the epsilon-caprolactone. The method comprises the following steps: carrying out polycondensation on a mixture of epsilon-caprolactone, 6-hydroxycaproic acid and a 6-hydroxycaproic acid linear oligomer / oligomer so as to convert the mixture into the 6-hydroxycaproic acid linear oligomer / oligomer, and depolymerizing the 6-hydroxycaproic acid linear oligomer / oligomer so as to convert the 6-hydroxycaproic acid linear oligomer / oligomer into epsilon-caprolactone or / and epsilon-caprolactone cyclic dimer. According to the method, cyclohexanone and hydrogen peroxide are used as reaction raw materials, the organic peroxide is prepared in a non-centralized manner in the whole route, and an organic solvent is not used, so that the combustion and explosion risks caused by the use of a large amount of organic peroxide and organic solvent are greatly reduced, and the yield of epsilon-caprolactone is improved through a polycondensation-depolymerization scheme.

The invention discloses a synthesis method of an unsaturated ketone or arone compound, which comprises the following steps: at a certain temperature, taking unsaturated hydrocarbon or aromatic hydrocarbon as a raw material, taking an N-hydroxyimide compound as a catalyst, adding an organic solvent for dissolving, introducing oxygen or air into a reaction solution under the irradiation of visible light, and carrying out oxidation reaction to obtain the unsaturated ketone or arone compound. And carrying out post-treatment separation to obtain the unsaturated ketone or arone. According to the method, air, oxygen-enriched gas or oxygen is used as a harmless oxidizing agent, visible light is used as an energy source to promote the reaction, and the method has the advantages that the reaction process is green and efficient, the cost is low, the dosage of the catalyst is small, and most of the catalyst can be recycled and reused; the atom economy is high.

The invention discloses a polyarylether sulfone polymer and a preparation method and application thereof. The preparation method of the polyarylether sulfone polymer comprises the following steps: carrying out condensation polymerization on a bisphenol compound and a dihalogen diphenyl sulfone derivative, boiling, washing and drying to obtain polyarylether sulfone resin. According to the polyarylether sulphone resin disclosed by the invention, by introducing benzoyl, the conjugation degree of a main chain of a polymer is increased, and the rigidity of the main chain is improved, so that the polyarylether sulphone resin has good thermal stability and dimensional stability; meanwhile, the hydrophilicity of the resin is improved due to the increase of carbonyl. The development and utilization prospects in the fields of sewage treatment, gas separation, solid electrolyte, battery diaphragms and the like are very wide. The invention aims to provide a novel high-temperature-resistant hydrophilic polyarylether sulfone resin and a preparation method thereof, i.e., a benzoyl group is introduced into a main chain structure of polyarylether sulfone, so that the structural rigidity of a polymer is improved, and the hydrophilicity is increased.

The invention discloses a preparation method and application of a reactive flame retardant containing double DOPO groups and nitrogen heterocycles, and the preparation method of the reactive flame retardant comprises the following steps: adding an amino compound R-NH2 and terephthalaldehyde into a reactor with a stirring device, adding a solvent, adding an acid to adjust the pH value to 6, then heating until the solvent is refluxed, keeping the refluxing temperature to react for a period of time, and cooling to room temperature to obtain the reactive flame retardant containing double DOPO groups and nitrogen heterocycles. Reaction liquid containing an imine intermediate product is obtained; then adding DOPO, controlling the reaction temperature to be the solvent reflux temperature, and keeping the reflux temperature to react for a period of time; after the reaction is finished, cooling, carrying out suction filtration, washing and drying to obtain a reaction type flame retardant containing double DOPO groups and nitrogen heterocyclic rings; the reaction formula is as follows: # imgabs0 # amino compound R-NH2 is 4-aminopyridine or 3-aminopyrazole, namely R is pyridyl or pyrazolyl. The synthesis and purification method of the flame retardant is simple, the reaction yield is high, and the flame retardant effect of epoxy resin can be remarkably improved by adding the flame retardant into bisphenol A epoxy resin through modification.

The invention provides a method for preparing pyroxasulfone through continuous oxidation by using a fixed bed catalyst, which comprises the following steps: respectively pumping a compound of formula I and hydrogen peroxide into a fixed bed catalyst reactor for reaction, and purifying the reaction liquid after the reaction is completed to obtain pyroxasulfone. The fixed bed catalyst reactor internally comprises a tungsten-containing catalyst loaded by a nano titanium silicalite molecular sieve, the mass content of the nano titanium silicalite molecular sieve is 25%-50%, and the mass content of the tungsten-containing catalyst is 50%-75%. The fixed bed catalyst reactor is used, the reuse efficiency is high, and the catalyst cost is greatly reduced. The amount of hydrogen peroxide used for oxidation is only the theoretically required amount, no hydrogen peroxide is left after the reaction, and the risk of the oxidation reaction is greatly reduced. The method is simple in purification treatment, high in reaction yield and low in three-waste yield.

The invention discloses a preparation method of octafluorocyclopentene, which comprises the following two steps of: firstly, reacting 4-cyclopentene-1, 3-diketone with a selective fluorine reagent in acetonitrile under the condition of reflux to generate a crude product second mixture, purifying the second mixture, and putting the purified second mixture into a second-step reaction to obtain the octafluorocyclopentene. Reacting with diethylamino sulfur trifluoride in dichloromethane to generate a third mixture; the method has the advantages of environment-friendly and simple reaction process, no generation of three wastes, low cost, easy obtaining, simple reaction process, mild reaction, no generation of waste gas pollution even if nitrogen protection is needed, easy operation, and suitableness for industrial production.

The invention discloses a preparation method of oxilafluorine, which comprises the following step: carrying out alkylation, deprotection, hydroxyethylation and salt forming reaction on a compound (II) to prepare the oxilafluorine as shown in a formula (I). The method has the advantages of low raw material cost, simple process operation, environmental friendliness, high reaction yield, high product purity and wide industrial prospect.

The invention discloses a synthesis method of dotenorad. The invention provides a preparation method of a compound B. The preparation method comprises the following step: reacting 3, 5-dichloro-4-hydroxybenzoic acid with a compound A to generate the compound B in an organic solvent under the action of a condensing agent. The preparation method provided by the invention is short in step, high in reaction yield, high in purity, low in three-waste generation amount, low in production cost and high in product quality, and is a green and environment-friendly preparation method. # imgabs0 #

The invention discloses a preparation method of 3-amino-2-fluorobenzoyl halide (formula V). The method comprises two routes: a route I and # imgabs 0 # or a route II and # imgabs 1 #, wherein R, R1 and R2 are defined in the specification.

The invention discloses a synthesis method of N-lauroyl sarcosine isopropyl ester, and belongs to the technical field of fine chemical engineering. The method comprises the following steps: adding N-lauroyl sarcosine, isopropanol and an activated carbon-solid acid composite catalyst into an esterification reaction kettle (the esterification reaction kettle is provided with a multiple dehydration device), carrying out esterification reaction, after the esterification reaction is completed, filtering reaction liquid to recover the composite catalyst, and distilling filtrate to recover isopropanol, so as to obtain isopropyl N-lauroyl sarcosine; according to the method, concentrated sulfuric acid is prevented from being used as a catalyst, the esterification rate is greatly increased, operation is easy, the method is suitable for industrial production, and the obtained N-lauroyl isopropyl sarcosinate is high in yield and good in color and luster.

The invention discloses an N-phenyl phenothiazine super-crosslinked polymer catalyst and a preparation method and application thereof.The method comprises the steps that Friedel-Crafts reaction is utilized, N-phenyl phenothiazine (I), dimethyl formal (II) and lewis acid are dissolved in a solvent, the mixture is stirred to react for 12-36 hours at the temperature of 60-120 DEG C, cooling and filtering are conducted, then extraction is conducted for 12-24 hours through a Soxhlet extractor, cooling and filtering are conducted again, and the N-phenyl phenothiazine super-crosslinked polymer catalyst is obtained. And drying the obtained solid to obtain the N-phenyl phenothiazine super-crosslinked polymer catalyst. The prepared N-phenyl phenothiazine super-crosslinked polymer catalyst can be applied to photocatalytic synthesis of 6-difluoromethyl phenanthridine derivatives, the reaction condition is mild, the catalytic efficiency is high, the selectivity is good, the catalyst can be recycled for multiple times, and the method is simple and easy to operate and has wide application potential.

The invention discloses a preparation method of fiazonetin, and belongs to the technical field of medicinal chemistry. According to the route, 2-halo-3-methylpyrazine which is low in price and easy to obtain is used as a raw material and sequentially reacts with hydrazine hydrate and orthoester, and then a hydrogenation reduction reaction is performed to generate a compound 4; carrying out chiral resolution or chiral separation on the compound 4 and carrying out condensation reaction on the compound 4 and p-fluorobenzoyl halide to obtain an intermediate compound 5 or 5'and a new intermediate compound 6; reacting the compound 6 with a halogenating reagent to obtain a compound 7; carrying out Suzuki coupling reaction on the compound 7 and a compound 8 to obtain a compound, namely, the compound of the formula A, namely, non-azonepan; according to the route, the raw materials are simple, easy to obtain and low in cost; the reaction is simple, the preparation efficiency is high, and the reaction yield of each step can be higher than 90%; no harsh reaction conditions exist, and operation is safe; post-treatment is simple and convenient, and environmental pollution is low. The method is suitable for large-scale production; a high-chiral product can be obtained, the chiral purity value of a final product is as high as 99.5%, and the method has relatively good market value and profound practical significance. # imgabs0 #

The invention belongs to the technical field of organic synthesis, and discloses a synthesis method of a disulfide compound. According to the invention, under the catalytic action of 1, 4, 7, 10, 13, 16-hexaoxacyclo-octadecane, halogenated hydrocarbon, sodium sulfide and sulfur react at the temperature of 50-60 DEG C to prepare the disulfide compound. The synthesis method of the disulfide compound has the advantages of being simple in process, small in catalyst dosage, mild in reaction condition, high in production efficiency, low in production cost, convenient for industrial production and the like, in addition, the reaction yield of the synthesis method can reach 94.8%-96.6%, and the purity of the obtained target product reaches up to 97.9%-99.3%. The method can be applied to preparation of the disulfide compound, and the obtained disulfide compound can be further applied to the fields of biomedicine, agriculture, chemical industry and the like.

The invention provides a synthesis method of saflufenacil, and belongs to the field of chemical synthesis. The preparation method comprises the following steps: reacting N-(2-chloro-4-fluoro-5-aminobenzoyl)-N '-isopropyl-N'-methyl sulfonamide serving as a raw material with chloroformate in a strong polar solvent, then directly adding alkali and ethyl 3-amino-4, 4, 4-trifluoro-2-butenoate into the reaction material, and carrying out cyclization reaction, so as to obtain the N-(2-chloro-4-fluoro-5-aminobenzoyl)-N '-isopropyl-N'-methyl sulfonamide. And carrying out methylation reaction on the cyclization reaction material and a methylation reagent to obtain saflufenacil. The selected reaction solvent is relatively single and easy to recover, so that the reaction operation is simple, the product yield is improved, and the method is suitable for industrial large-scale production and has a wide application prospect.

The invention belongs to the technical field of lithium ion batteries, and particularly relates to an organic polymer containing carbonyl and imine as well as a preparation method and application of the organic polymer. Aiming at the problems of insufficient solvent resistance and limited inherent conductivity of a lithium ion battery positive electrode material, the invention designs and synthesizes an organic polymer with rich redox active sites and an expanded pi conjugated structure. The organic polymer containing carbonyl and imine provided by the invention has reversible lithium ion storage, relatively high actual specific capacity, excellent cycle stability, excellent rate capability and high energy density and power density. In the synthesis of the organic polymer provided by the invention, experimental raw materials are cheap and easily available, the preparation method is simple, the reaction yield is relatively high, large-scale application of the material in the field of lithium ions is facilitated, and the material has a wide application prospect.

The application belongs to the technical field of organic synthesis, and specifically provides a preparation method of Mal-PEG2-CH2COOH, comprising the following steps: S1, reacting AEEA with maleic anhydride to generate an intermediate, wherein the intermediate is (Z)-2-(2-(N-hydroxyethyl)hydroxyethyl)carboxymethyl)maleic acid monoamide; and S2, performing ring closure reaction on the intermediate to generate Mal-PEG2-CH2COOH. According to the preparation method of the embodiment of the application, the open ring-closure step-by-step synthesis strategy is adopted, so that the harsh reaction condition of high temperature and acid is avoided, the preparation cost is reduced, the overall reaction yield is improved, and the three-waste discharge and environmental pollution are reduced.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of 2-(4-bromophenyl) norcamphane. According to the invention, the proper catalyst is selected to promote the norbornene to be directly added with the bromobenzene Grignard reagent, so that the use of expensive raw materials is avoided, the reaction difficulty is reduced, and the reaction can be smoothly carried out, thereby effectively improving the reaction yield of the 2-phenyl norcamphane. According to the bromination reaction of the 2-phenyl norcamphane, proper catalysts and reaction conditions are selected, and the selectivity of para-products is improved, so that the product yield of the 2-(4-bromophenyl) norcamphane is improved.

The invention discloses a synthesis method of a 1, 3-benzoxazine compound. Belongs to the technical field of organic compound process application. 1, 3-benzoxazine is a key skeleton structure of many drug molecules and has a wide application prospect. Specifically, a series of 1, 3-benzoxazine compounds are obtained by catalyzing o-hydroxyphenyl substituted p-methylene quinone and ketimine to react in a solvent by taking binaphthol phosphate as a catalyst through a Diels-Alder hybrid reaction. According to the method, the product with high yield is rapidly obtained from cheap raw materials through simple operation under mild reaction conditions, and the method is suitable for industrial large-scale production.

The invention discloses a method for improving the synthesis reaction rate of lithium difluorophosphate, which comprises the following steps: in an organic solvent, taking lithium hexafluorophosphate, chain siloxane and / or cyclic siloxane as raw materials, and adding water accounting for 0.1-5.0% of the molar weight of the lithium hexafluorophosphate to prepare the lithium difluorophosphate. The method disclosed by the invention is simple in process and mild in reaction condition, and the reaction yield can be increased while the reaction time is greatly shortened.