110results about "Oximes preparation" patented technology

The invention discloses a copper-based catalyst for catalyzing partial hydrogenation of nitrocyclohexane to prepare cyclohexanone-oxime as well as a preparation method and application of the copper-based catalyst. The catalyst comprises a main active component and an auxiliary active component, the main active component is copper, the auxiliary active component is selected from one or more of titanium, vanadium, chromium, molybdenum, zirconium, cadmium, indium, tin, antimony, niobium, silver, iron, zinc, magnesium, aluminum, bismuth, manganese, lanthanum, gold or lead, the total molar ratio of the copper to the auxiliary active component is (100-1): 1, and the catalyst is prepared by adopting a coprecipitation method or a supported impregnation-coprecipitation method. And the process is simple and green. Under mild conditions, the catalyst can realize the conversion rate gt of nitrocyclohexane; the selectivity of cyclohexanone-oxime is greater than or equal to 99%, and the method is obviously superior to the existing non-noble metal system, and is low in cost, good in stability and suitable for industrial production of green synthesis of caprolactam.

The present invention relates to the preparation of cyantraniliprole, comprising the preparation of 8-methyl-2,4-dioxo-1,4-dihydro-2H-benzo[d][1,3]oxazine-6-carbonitrile key intermediate via 2-amino-5-((hydroxyimino)methyl)-3-methylbenzoic acid. Wherein hydroxylamine attacks a benzylic formyl group, to obtain the 2-amino-5-((hydroxyimino)methyl)-3-methylbenzoic acid, that undergoes simultaneously or by consecutive steps dehydrogenation and cyclization to obtain the benzo[d][1,3]oxazine group and the cyano group of the desired product. In addition, an improved method for the synthesis of the benzylic formyl group is also displayed.

The invention relates to a method for preparing ketoxime compounds, which comprises the following steps: contacting a ketone compound, a catalyst and an ammonia source in a liquid-phase medium to obtain a reaction mixture, and releasing ammonia gas from the ammonia source; the catalyst comprises a carrier and active metal loaded on the carrier, the active metal comprises IB group metal and VIII group metal, and the carrier comprises a titanium silicalite molecular sieve; introducing the first raw material gas and the second raw material gas into the reaction mixture to be in contact with a catalyst for in-situ reaction to obtain a reaction product containing the ketoxime compound; wherein the first feed gas comprises hydrogen, and the second feed gas comprises oxygen. According to the method, hydrogen and oxygen are used as reaction raw material gases, ketoxime is prepared through in-situ ammoximation of ketone compounds, the safety problem caused by production, use, storage and transportation of hydrogen peroxide is solved, and the method is simple in process and environmentally friendly.

The application provides a synthesis method of p-benzoquinone dioxime. The synthesis method comprises the following steps: (1) adding solid acid into an ethanol solution of phenol to obtain a mixed solution A, then vacuumizing and filling with inert gas; dissolving nitrite into ethanol, uniformly mixing to obtain an ethanol solution of nitrite, then vacuumizing and filling with inert gas; in an inert gas atmosphere, adding the ethanol solution of nitrite into the mixed solution A dropwise to perform nitrosation reaction, to obtain a reaction liquid B; in the inert gas atmosphere, adding an ethanol solution of hydroxylamine into the obtained reaction liquid B to perform oximation reaction; after the reaction is completed, filtering the obtained reaction liquid C, performing reduced pressure distillation on the obtained filtrate, and performing washing, filtering and drying on the obtained residual liquid of the reduced pressure distillation, to obtain p-benzoquinone dioxime. The method provided by the application reduces the occurrence of side reactions, improves the conversion rate of the reaction, and improves the yield and purity of p-benzoquinone dioxime.

The invention discloses a synthesis method of 9-dichloromethylene-5-amino-benzonorbornene and an intermediate product, the synthesis method comprises the following steps: firstly, synthesizing a cyclization compound 1 as shown in a formula 1 from a cold solution of 6, 6-dichlorofulvene and 1, 4-benzoquinone under the action of a solution of a catalyst I, carrying out oximation reaction on the cyclization compound 1 prepared in the step a and hydroxylamine salt under an alkaline condition, and carrying out post-treatment to obtain the 9-dichloromethylene-5-amino-benzonorbornene. Under the action of a catalyst II, adding the oximate 2 prepared in the step b into a closed container, carrying out hydrogenation reduction to obtain 9-dichloromethylene-5-amino-benzo norbornene, and directly treating the reduction product with acid to obtain 9-dichloromethylene-5-amino-benzo norbornene, namely the 9-dichloromethylene-5-amino-benzo norbornene, namely the 9-dichloromethylene-5-amino-benzo norbornene. According to the method, the cyclization compound is oximated firstly, then the residual carbonyl and two double bonds on the ring are subjected to one-step reduction through catalytic hydrogenation, the working procedure is optimized, meanwhile, reduction by using expensive sodium borohydride is avoided, the method is short in synthesis route and suitable for industrialization, and the production cost is reduced.

The invention belongs to the technical field of preparation of herbicides, and particularly relates to a preparation method of tralkoxydim. The preparation method comprises the following steps: carrying out ethylation reaction on 3-hydroxy-5-(2, 4, 6-trimethylphenyl)-2-propoximido-cyclohex-2-ene-1-ketone and halogenated ethane under an alkaline condition, so as to prepare tralkoxydim. According to the method, the use of ethoxyamine hydrochloride or ethoxyamine in the traditional process is innovatively avoided, the raw material cost is reduced, the ethylation reaction is carried out by using halogenated ethane, the reaction raw materials are cheap and easy to obtain, meanwhile, single sodium / potassium halide wastewater is produced, the wastewater treatment process is greatly simplified, meanwhile, the generation of carnallite wastewater and carnallite-containing solid waste is eliminated, and the method is suitable for industrial production. The method has the advantages of environmental protection, economy and simple process, and is suitable for industrial large-scale production.

This invention provides a method for preparing dibenzoyl-p-benzoquinone dioxime using a microchannel reactor. The method includes the following steps: 1,3-dicyclohexylcarbodiimide and a catalyst are mixed uniformly and preheated to obtain a premix; a chloroform solution of p-benzoquinone dioxime, a chloroform solution of benzoic acid, and the premix are simultaneously introduced into the microchannel reactor for reaction; the resulting reaction solution is subjected to vacuum distillation, washing, filtration, and drying to obtain dibenzoyl-p-benzoquinone dioxime. The synthesis method of this invention features high reaction conversion rate, high production efficiency, few side reactions, and high safety. The obtained dibenzoyl-p-benzoquinone dioxime product has stable quality. Furthermore, the organic solvent used can be recovered and reused after vacuum distillation, overcoming the problems of inaccurate temperature control, poor safety, numerous side reactions, and difficult waste treatment in traditional processes. This provides a new approach for the synthesis of dibenzoyl-p-benzoquinone dioxime.

The embodiment of the present application provides a kind of spherical dihydroxy glyoxime and its preparation method and energetic material.The method comprises the following steps: hydrochloric acid solution and dihydroxy glyoxime metal salt suspension are simultaneously added into reaction bottom liquid containing regulator, crystallization reaction is carried out, and crystal suspension is obtained;The crystal suspension is filtered, and the spherical dihydroxy glyoxime is obtained.The method is used to achieve the effect of providing the flowability and bulk density of spherical dihydroxy glyoxime.

A method for preparing the insecticide N-(1-methylcyclopropyl)-2-(3-pyridinyl)-2H-indazole 4-carboxamide is disclosed. A method for preparing the intermediate N-(1-methylcyclopropyl)-2-(3-pyridinyl)-2H-indazole 4-carboxamide is also disclosed.

The invention provides an aldehyde insect pheromone derivative, which takes a compound containing at least one primary amine group as a carrier, and aldehyde insect pheromone forms an imine derivative with the compound through chemical reaction. The invention also provides a preparation method, application and a release method of the aldehyde insect pheromone derivative. According to the aldehyde insect pheromone derivative provided by the invention, aldehyde insect pheromones are treated in a chemical reaction manner, the stability of the aldehyde insect pheromones can be remarkably improved, slow release and controlled release of the pheromones can also be realized, the carrier material is wide in source, more in selectivity, convenient and economical, and in addition, the aldehyde insect pheromone derivative has good application prospects. The aldehyde insect pheromone derivative provided by the invention can also realize combined fixation and release of various pheromones, so that trapping, prevention and control of various insects can be realized.

The invention provides an aryl alkyl ketoxime derivative as well as a preparation method and application thereof, and relates to the field of aryl oxime derivatives. The preparation method of the aryl alkyl ketoxime derivative comprises the following steps: by taking potassium formate as an additive, carrying out free radical reaction on a compound I and a compound II under ultraviolet irradiation in the presence of tert-butyl nitrite to obtain the aryl alkyl ketoxime derivative, the compound I is substituted iodobenzene or iodopyridine; the compound II is substituted styrene or thienyl ethylene; wherein a hydrogen atom transfer / single electron transfer relay sequence is utilized to activate a compound I, and tert-butyl nitrite is adopted as a bifunctional reagent, and is used as a hydrogen atom transfer reagent and an oxime source. According to the preparation method of the aryl alkyl ketoxime derivative, pre-functionalization is not needed, a reaction substrate is wide in universality and good in compatibility, reaction conditions are mild, operation is easy and convenient, a target product can be efficiently and rapidly prepared on the premise of high yield, and a new way is provided for oxime synthesis.

The invention belongs to the technical field of pesticides, and particularly relates to carvone oxime ether compounds as well as a preparation method and application thereof. The carvone oxime ether compound has a chemical structure as shown in a formula (I). The invention provides a series of brand new carvone oxime ether compounds for the first time. In addition, the invention also provides a synthetic method of the carvone oxime ether compound, the product prepared by the synthetic method is high in yield and easy to separate, and the synthetic method is an optimal synthetic route for preparing the carvone oxime ether compound; the carvone oxime ether compound can be used for controlling stored grain pests, especially controlling tribolium castaneum of wheat, rice, corn, sorghum, peanuts, oilseed rape, soybeans and the like, and has the characteristics of high acting speed and high activity. The carvone oxime ether compound disclosed by the invention can be used as a stored grain pest control fumigant, has good development potential, and provides a new thought for developing and creating a new green fumigant.

The utility model relates to the field of production devices of organic chemical raw materials, and discloses a cyclohexanone oxime preparation device. The device comprises a reaction unit, a washing unit 6, a product separation unit 7 and an extraction unit 8, wherein the reaction unit comprises at least one reactor 1, a reaction cooler 2, a catalyst separator 3 and a membrane filter 4 which is arranged in the catalyst separator 3 or is communicated with a water phase outlet of the catalyst separator 3; the reactor 1 is provided with a raw material inlet communicated with a circulating catalyst slurry pipeline 10 and a hydrogen peroxide inlet communicated with a hydrogen peroxide supply device, and the circulating catalyst slurry pipeline 10 is provided with a cyclohexanone inlet and an ammonia inlet. The device disclosed by the utility model obviously prolongs the service life of the catalyst, effectively removes impurities in cyclohexanone oxime, and has higher cyclohexanone conversion rate and cyclohexanone oxime selectivity.

The application discloses a preparation method of a non-conjugated functionalized olefin compound, and the method is carried out in a cobalt / photocatalysis dual catalytic system which is composed of a cobalt catalyst, a ligand, a photocatalyst, a hydrogen source, a base and a solvent. β The target product is efficiently and selectively synthesized through reaction of an ethylenic compound or a halogenated compound or an electron-deficient olefin represented by formula (2) with acetylene as a C2 synthetic unit. The application adopts a cobalt / photocatalysis dual catalytic synergistic mechanism, has mild conditions (normal temperature and pressure, visible light driving), uses water as a green hydrogen source, uses acetylene as a cheap C2 source, has high atom economy, has good substrate universality, and the compound represented by formula (1) is easy to be prepared through Friedel-Crafts acylation or is commercially available, and the compound represented by formula (1) is easy to generate the compound (III) represented by formula (2) under the action of a base. The obtained non-conjugated olefin is a key intermediate for synthesizing high-value-added fine chemicals such as fragrances and insect pheromones, and has wide application prospects.

The invention discloses a method for co-production of 2, 4-dichloro-5-fluoroacetophenone and hydroxylamine hydrochloride, and belongs to the technical field of organic chemical industry, 2, 4-dichlorofluorobenzene is used as a raw material, alkylation and reaction with tert-butyl nitrite are performed to generate oxime, and then hydrochloric acid hydrolysis is performed to generate 2, 4-dichloro-5-fluoroacetophenone and hydroxylamine hydrochloride; according to the method, co-production of the 2, 4-dichloro-5-fluoroacetophenone and the hydroxylamine hydrochloride is innovatively realized, not only are high yield and high purity of the target product 2, 4-dichloro-5-fluoroacetophenone ensured, but also the nitrogen element in the reaction is recycled and converted into the hydroxylamine hydrochloride with high additional value, and the atom economy is remarkably improved; according to the method, the operation process is greatly simplified, the use of dangerous reagents is avoided, and the intrinsic safety and environmental friendliness of the process are improved from the source; the method is simple to operate, safe and environment-friendly, the production cost is effectively reduced, and the market competitiveness of the product is enhanced.

The invention relates to a preparation method of a trifloxystrobin intermediate (E)-2-(2-bromomethyl phenyl)-2-methoxyimino methyl acetate, and belongs to the technical field of organic chemistry. The method comprises the following steps: by taking a trifloxystrobin intermediate (E)-2-(2-bromomethyl phenyl)-2-methoxyimino methyl acetate containing dibromo impurities as a raw material and an organic solvent I as a reaction medium, carrying out debromination reaction at 5-60 DEG C by using phosphite, desolventizing and extracting a reaction solution, and crystallizing to obtain the high-purity (E)-2-(2-bromomethyl phenyl)-2-methoxyimino methyl acetate. According to the method disclosed by the invention, the dibromo impurity of the trifloxystrobin intermediate is subjected to debromination treatment by adopting the phosphite, so that the dibromo impurity is converted into the trifloxystrobin intermediate. By adopting the method provided by the invention, the conversion time of the dibromo impurity can be obviously shortened, the content and the yield of the trifloxystrobin intermediate obtained by conversion are both higher than 95%, and the reaction efficiency and the quality of the intermediate are greatly improved.

The application provides a preparation method of dibenzoyl-p-benzoquinone dioxime. The method comprises the following steps: (1) adding a heteropoly acid catalyst into an ethanol solution of p-benzoquinone dioxime to obtain a mixed solution; (2) adding an ethanol solution of benzoic acid into the obtained mixed solution, and then performing a reaction; after the reaction is completed, filtering the obtained reaction liquid, drying and screening the obtained filter residue to obtain dibenzoyl-p-benzoquinone dioxime. The method uses p-benzoquinone dioxime and benzoic acid as raw materials, uses ethanol as a reaction solvent, uses a heteropoly acid as a catalyst for a condensation reaction, and synthesizes dibenzoyl-p-benzoquinone dioxime in one step. The solvent ethanol used in the method can be recovered and reused through reduced pressure distillation, and the catalyst heteropoly acid can be recycled and reused after being filtered, so that the output of acidic production wastewater is reduced, the generation of strong corrosive hydrogen chloride gas is avoided, and the green environmental protection requirement is met.

The present application provides 1H-imidazo[4,5-h]quinazoline compounds of Formula (I). The compounds are broad-spectrum inhibitors with strong activity against FLT3 kinase and are useful in the treatment of cell proliferative disorders.

The invention relates to the field of production of caprolactam by Beckmann rearrangement of cyclohexanone-oxime, and discloses a gasification method and system of cyclohexanone-oxime. The method comprises the following steps: gasifying a circulating cyclohexanone oxime liquid phase, inert gas and a first solvent in a gasifier, and then carrying out gas-liquid separation to obtain a first gas-phase material and a liquid-phase material; (2) returning part of the liquid-phase material to the gasifier for gasification; (3) mixing the rest of the liquid-phase material with a second solvent to obtain a mixed solution; then feeding the mixed solution to a fluidized bed to be in contact with solid particles for secondary gasification to obtain solid particles attached with heavy substances and a second gas-phase material; carrying out Beckmann rearrangement reaction on the first gas-phase material and the second gas-phase material; wherein the temperature of the solid particles is at least 20 DEG C higher than that of the mixed liquid. The method provided by the invention can reduce the throwing amount of heavy impurities, improve the utilization rate of cyclohexanone-oxime, reduce the unit consumption of cyclohexanone-oxime, and improve the activity and service life of the catalyst.

The application discloses a preparation method of an amido pyrazole compound and a method for preparing sildenafil by using the same. The amido pyrazole compound is shown as formula I. The compound of formula I is prepared by using 2-pentanone as an industrial chemical, and can be used for synthesizing sildenafil which is a selective inhibitor of type 5 phosphodiesterase (PDE5). The method has the advantages of easy availability of raw materials, simple operation, avoidance of nitration reaction, avoidance of safety hidden dangers caused by the nitration reaction from a technical source, and avoidance of environmental protection pressure caused by a large amount of nitration waste liquid, and is suitable for development into a green and sustainable production process of sildenafil bulk drug.

This invention discloses a kinetically controlled method for preparing hierarchical porous molecular sieves, belonging to the field of catalyst preparation technology. It employs a two-step crystallization method: first, nucleation occurs at low and ultra-low H2O / SiO2 molar ratios; then, after the low-temperature phase, water is added, followed by rapid growth at high temperature and high H2O / SiO2 molar ratios. The solid-phase and liquid-phase crystallization mechanisms in the synthesis system work in succession to prepare hierarchical molecular sieves. This invention, without adding any mesoporous pore-forming agents, only modulates the crystallization temperature and the H2O / SiO2 molar ratio of the synthesis system to kinetically control the crystallization mechanism, resulting in molecular sieves with higher catalytic performance than those obtained using traditional methods. Furthermore, it overcomes the drawbacks of traditional hierarchical porous molecular sieve preparation processes, such as high cost, high calcination energy consumption, poor mesopore connectivity, and severe contamination from pore-forming agents.

The invention discloses a cyclohexene diketone lactic acid oxime ether compound as shown in a formula I, and a stereoisomer, a tautomer, a solvate or a pesticide acceptable salt thereof, and in the formula I, R1-R4 are defined in the specification. The compound as shown in the formula I contains a specific lactic acid or lactic acid derivative structural fragment, has very high herbicidal activity and safety, and has a good control effect on resistant weeds at the same time.

The present application relates to the technical field of organic chemical intermediates purification, in particular to a method and device for cis-trans isomerization conversion of 4-halo-2-methoxy imino acetoacetic acid ethyl ester. After cooling, 4-halo-2-methoxy imino acetoacetic acid ethyl ester is mixed with sodium chloride brine to form crystal slurry; then the crystal slurry is discharged into a crystal conversion kettle for aging; after aging, the crystal slurry is heated, extracted and centrifuged, and the organic phase is collected to obtain 4-halo-2-methoxy imino acetoacetic acid ethyl ester. Through the continuous process of "low-temperature brine crystallization enrichment-crystal conversion aging directional conversion-microwave rapid heating to prevent reverse conversion-two-stage extraction centrifugation purification-brine circulation to reduce cost", the content of cis-4-halo-2-methoxy imino acetoacetic acid ethyl ester is stably increased to 92-95%, and the production cost and environmental risk are reduced.

The invention relates to a benzophenone oxime ester photoinitiator and a preparation method thereof, and the structure of the benzophenone oxime ester photoinitiator compound is as shown in formula (1), specifically as shown in the specification. According to the benzophenone oxime ester photoinitiator provided by the invention, oxime group (= N-OH) and ester group (-COOR) functional groups are introduced, so that the molecular structure of a benzophenone compound is increased, the characteristic that the benzophenone compound serving as the photoinitiator is easy to yellow is improved, the solubility is improved, and meanwhile, the benzophenone oxime ester photoinitiator has the advantages of high curing speed and the like of an oxime ester cracking type photoinitiator.

The invention belongs to the technical field of organic synthesis, and particularly relates to a chloroamine synthesis method which comprises the following steps: S1, mixing a hydroxylamine sulfate aqueous solution and methyl acetate, and then dropwise adding a NaOH aqueous solution to react for 1-2 hours; s2, adding trans-1, 3-dichloropropene and the sulfonated niobium-doped TS-1 molecular sieve, uniformly mixing, heating to 60-70 DEG C, and carrying out etherification reaction for 5-6 hours to generate an intermediate product; s3, adding hydrochloric acid into the intermediate product, fully stirring, and carrying out reflux reaction at 60-70 DEG C for 2-3 hours; s4, organic matter is separated through reduced pressure distillation, then a NaOH aqueous solution is added to adjust the pH to be larger than 9, extraction is conducted, the extraction agent is removed through reduced pressure distillation, and chloramine is obtained. According to the synthesis method provided by the invention, the selectivity of the chloro-amine is 99% or above, the yield of the chloro-amine is 98% or above, the production efficiency of the chloro-amine can be effectively improved, and the synthesis method is suitable for industrial application.

This invention relates to the field of pharmaceutical intermediates, and in particular to a method for synthesizing chiral indane. The method uses indane as a raw material, synthesizes an oxime, then an enamine, and subsequently synthesizes the trans-chiral indane via an asymmetric hydrogenation reaction using a ruthenium chiral bisphosphine catalyst, achieving high yield and high stereoselectivity. The advantages of this invention are: in the asymmetric hydrogenation reaction of the enamine, the trans-chiral indane is obtained with a content greater than 97%, an ee of 95%, and a yield greater than 90%; the catalyst is readily available; the operation is simple; the raw materials are readily available; there is minimal pollution from waste; and energy consumption is low, making it suitable for industrial production.

Process for the preparation of propan-2-imine-substituted phenyls / oxime ethers, in particular to the preparation of 1-(2,4,6-trichlorophenyl)-propan-2-one oxime and N-methoxy-1-(2,4,6-trichlorophenyl)- propan-2-imine.

The application belongs to the technical field of medicine, and particularly relates to a muscone derivative, a preparation method and application thereof. The muscone derivative cyclopentadecanedione monoxime has obvious advantages over muscone and other derivatives in improving the MCAO rat mNSS score, microcirculation blood flow, reducing the cerebral infarction rate, the cortical and hippocampal neuron necrosis rate, and the brain water content, and increasing the SOD and CAT contents of the rat brain tissue which are abnormally reduced due to ischemia, and is a potential effective drug for cerebral ischemia-reperfusion injury.

The application belongs to the technical field of molecular sieve material preparation, and provides a high-stability multi-level pore FER-type titanium-silicon molecular sieve and a preparation method and application thereof.The preparation method of the FER-type titanium-silicon molecular sieve comprises the following steps: immersing a kanemite into a fluorosilicic acid solution for activation, then modifying the activated kanemite by using tetraethyl orthosilicate to obtain a modified silicon source; mixing the modified silicon source, a titanium source, a composite template agent, a crystal seed, a silane coupling agent and water to obtain a gel, and then crystallizing to obtain a precursor; calcining the precursor and then performing acid modification to obtain a FER topology structure; immersing the FER topology structure into an ammonium dihydrogen phosphate solution for reaction, and then sequentially drying and calcining to obtain the FER-type titanium-silicon molecular sieve.The preparation process parameters are mild, each link is synergistically controllable, special and expensive equipment is not needed, and the industrialized scale production is easy to realize.

The present application provides compounds of Formula (I): Formula (I) or a stereoisomer, tautomer, or pharmaceutically acceptable salt or solvate thereof, wherein all variables are as defined herein. These compounds are selective LPA receptor inhibitors.