27 results about "Oxime ether" patented technology

The invention provides a bromo-oxime ether content detection method which is characterized by comprising the following steps: adding a bromo-oxime ether reaction solution into an anhydrous aprotic polar solvent, adding a sodium alkoxide solution for reaction, and purifying to obtain a standard sample of a bromo-oxime ether sodium alkoxide derivative; adding the bromo-oxime ether reaction solution into an anhydrous aprotic polar solvent, and adding a sodium alkoxide solution for reaction to obtain a to-be-detected sample of the bromo-oxime ether sodium alkoxide derivative; and analyzing the standard sample and the sample to be detected by adopting a high performance liquid chromatography external standard method to obtain the content of bromo-oxime ether in the bromo-oxime ether reaction liquid. The method is high in detection accuracy, good in repeatability and suitable for being applied to the scenes of laboratory research and development, factory production and the like.

The invention belongs to the field of medicines, and relates to an oxime ether spinosad derivative as well as a preparation method and application thereof. The oxime ether spinosad derivative is a compound as shown in a structural general formula (I), a salt thereof or an optical isomer thereof, wherein R1 is selected from NR8R9, a C5-C8 nitrogen-containing heteroaromatic ring, a C3-C7 nitrogen-containing aliphatic ring, a substituted C5-C8 nitrogen-containing heteroaromatic ring and a substituted C3-C7 nitrogen-containing aliphatic ring. The oxime ether spinosad derivative disclosed by the invention has strong anti-tumor activity and can be used as a potential drug for treating tumor diseases.

This invention discloses a class of aryl acetone oxime ether derivatives and their applications, belonging to the field of medicinal chemistry. The derivatives are compounds represented by general formula (I) or pharmaceutically acceptable salts thereof, exhibiting excellent regulatory activity against the S1P1 receptor, as well as excellent pharmacokinetic properties and anti-inflammatory efficacy. This invention also discloses pharmaceutical compositions comprising the derivatives and their application in the preparation of drugs for the prevention and / or treatment of autoimmune diseases, which can be used for the treatment of diseases such as multiple sclerosis and ulcerative colitis. General formula (I).

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.

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 present application relates to the technical field of antibacterial drugs, and specifically discloses a pleuromutilin derivative and a use thereof, wherein the pleuromutilin derivative has a structure of being connected to a side chain of C14 of pleuromutilin by a mercaptoethylamine, piperazine or oxygen atom from a dihydroflavone or oxime ether derivative thereof. The present application introduces dihydroflavone (naringenin and hesperetin) and oxime ether derivatives thereof having antibacterial effects into the side chain of C14 of pleuromutilin by taking pleuromutilin as a raw material. The dihydroflavone and oxime ether derivatives thereof have great potential as an advantageous structural unit due to their unique C6-C3-C6 basic skeleton (C2 and C3 are single bonds) and extensive antibacterial activity. The dihydroflavone and oxime ether derivatives thereof are combined with pleuromutilin to synthesize a plurality of dihydroflavone pleuromutilin derivatives having excellent antibacterial activity. The present application provides a new choice for designing a new generation of pleuromutilin derivatives by a hybrid strategy, improving drug properties while improving activity, and providing an anti-infective drug.

This invention provides a method for preparing green oxime ester, comprising the following steps: adding dichloroethane and m-trifluoromethylacetophenone oxime to a synthesis reactor, stirring until dissolved, then adding granular sodium hydroxide, stirring at 22℃-33℃ for 0.5h-2h, then adding potassium carbonate and tetrabutylammonium bromide, cooling, and then adding brominated oxime ether for a condensation reaction, adding water after the reaction and separating the layers, removing the lower oil phase under vacuum to remove dichloroethane, adding 90% methanol for crystallization, filtering, washing, and drying to obtain oxime ester. This invention uses dichloroethane throughout the condensation, bromination, and extraction steps, simplifying the solvent system and reducing residues and energy consumption; the combination of granular sodium hydroxide and potassium carbonate ensures efficient deprotonation and in-situ dehydration, suppressing side reactions and thus improving yield and purity; in the preparation of brominated oxime ether, n-butanol is recycled and crystallized in a controlled manner, achieving reduced consumption and safety, while saline wastewater is neutralized and recovered, effectively reducing chemical oxygen demand emissions.

The invention belongs to the field of medicines, and relates to application of an oxime ether spinosad derivative in treatment of citrullinemia. The oxime ether spinosad derivative is a compound as shown in a structural general formula (I), a salt thereof or an optical isomer thereof, wherein R1 is selected from NR8R9, a C5-C8 nitrogen-containing heteroaromatic ring, a C3-C7 nitrogen-containing aliphatic ring, a substituted C5-C8 nitrogen-containing heteroaromatic ring and a substituted C3-C7 nitrogen-containing aliphatic ring.

The present application relates to a kind of preparation method of pesticide intermediate.The pesticide intermediate is oxime ether.In existing production process, dimethyl sulfate, halogenated methane and other methylating reagents are used.However, these reagents are highly toxic, harmful to the health of employees, and also cause adverse effects on the ecological environment.The present application opens up a green synthesis process, and uses low-toxic methylating reagents to complete methylation.In esterification reaction, a new esterification method is used, and highly toxic or dangerous materials such as dimethyl sulfate, concentrated sulfuric acid or hydrogen chloride gas are abandoned, which have great environmental impact.The method is healthy and environmentally friendly, safe to operate, reduces environmental pollution and lowers production costs.

The present invention relates to novel processes for the enantioselective iridium-catalysed hydrogenation of oximes and oxime ethers to provide compounds of formula (II) and salts thereof formula (I) and (II).

The invention belongs to the technical field of chemical synthesis, and provides a method for synthesizing alkoxyamine hydrochloride by oxime ether hydrolysis. The method for synthesizing the alkoxyamine hydrochloride by oxime ether hydrolysis comprises the following steps: adding a solvent into a hydrolysis system of oxime ether and hydrochloric acid, uniformly mixing, and carrying out reduced pressure hydrolysis. According to the present invention, the specific type of the solvent is added to the hydrolysis system of the oxime ether and the hydrochloric acid, such that the oxime ether and the hydrochloric acid can be completely mixed, the acidification is complete, the hydrolysis is easily performed, the side reaction is reduced, the yield of the alkoxyamine hydrochloride is improved, the yield reaches more than 80%, and the purity reaches more than 90%.

This invention belongs to the field of organic synthesis technology and discloses a method for preparing trans-3-chloro-2-propenylhydroxylamine hydrochloride. The method involves adding trans-1,3-dichloropropene to a ketoxime, a base, a phase transfer catalyst, and a first solvent for etherification. After the reaction, the mixture is first extracted with an extractant, and the resulting oil phase is then distilled to obtain the oxime ether. The oxime ether, an aqueous hydrochloric acid solution, and a second solvent are mixed and subjected to vacuum distillation in a distillation column to obtain trans-3-chloro-2-propenylhydroxylamine hydrochloride. This invention avoids the use of an aqueous base in the etherification stage, effectively preventing the hydrolysis of the ketoxime. The purified oxime ether obtained in the etherification step is purified by distillation, significantly reducing side reactions during the subsequent hydrolysis. Adding a solvent during the hydrolysis stage allows for better mixing of the aqueous hydrochloric acid solution and the oxime ether, resulting in more uniform acidification, a more complete reaction, and improved conversion and selectivity.

The invention provides a method for synthesizing oxime ether from an amino compound in one step and the obtained oxime ether. The method comprises the following steps: 1) taking a compound a and 3, 5-di-tert-butyl o-benzoquinone, mixing, adding an organic solvent, and stirring at room temperature for 0.5-1.5 h to obtain a mixture; 2) taking O-substituted hydroxylamine and an organic acid solution with the volume concentration of 30-70%, mixing, adding into the mixture, and reacting at room temperature for 1-16 hours to obtain a head product; and 3) removing the organic solvent in the head product to obtain a residue, and purifying to obtain a target product c. According to the present invention, the amino compound is adopted as the raw material, the oxime ether is synthesized in one step through the one-pot method under the action of the 3, 5-di-tert-butyl-o-benzoquinone and the O-substituted hydroxylamine, such that the process is short, the selectivity is high, the intermediate product does not need to be separated, the synthesis time is saved, the yield is high, the applicable substrate is wide, the application potential is large, the reaction condition is mild, the reaction can be completed at the room temperature, the safety is high, and the cost is low; the method is suitable for large-scale production.

The invention belongs to the technical field of chemical synthesis of medicines, and particularly relates to a preparation method of avibactam sodium. According to the method, (2S, 5R)-trans-5-hydroxypiperidine-2-formic acid is taken as a starting raw material, hydroxyl in the (2S, 5R)-trans-5-hydroxypiperidine-2-formic acid is efficiently and selectively converted into hydroximido by adopting an electrochemical method, the condition is mild, the method is environment-friendly, and the pollution problem caused by using an equivalent metal reducing agent or an oxidizing agent in a traditional chemical method is avoided; after O-benzyl oxime ether is constructed, a (2S, 5R) absolute configuration required by avibactam sodium is constructed and maintained through stereoselective reduction and efficient amination. From (2S, 5R)-trans-5-hydroxypiperidine-2-formic acid to avibactam sodium, the route design is ingenious, the steps are shorter, and a novel, simple and efficient synthesis route is provided for synthesis of avibactam sodium.

The present invention belongs to the technical field of organic synthesis, and particularly relates to a method for preparing 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-methoxy oxime ether. The method comprises the following steps: (1) chlorination reaction: adding a chlorinating agent into aniline as a raw material in a solvent at 0-10°C, and performing a chlorination reaction to obtain 2,4,6-trichloroaniline; (2) coupling reaction: subjecting 2,4,6-trichloroaniline, isopropenyl acetate and a catalyst to a coupling reaction in a solvent under the initiation of nitroxyl ions, so as to obtain 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone; (3) oximation reaction: subjecting 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone and hydroxylamine hydrochloride to an oximation reaction in a solvent under the action of an alkali, so as to obtain 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-oxime; and (4) methylation reaction: subjecting 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-oxime and chloromethane to a methylation reaction in a solvent under the action of an alkali, so as to obtain 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-methoxy oxime ether.

The application belongs to the technical field of propagation of Artocarpus heterophyllus, and particularly relates to a high-branch layering propagation method of Artocarpus heterophyllus. The high-branch layering propagation method of Artocarpus heterophyllus comprises the following steps: S1. selecting a single branch with a healthy growth state and performing ring peeling; S2. after the cambium is scraped off, a plastic film is wrapped around the upper end of the ring peeling; S3. after the plastic bag is longitudinally cut, the plastic bag is wrapped around the ring peeling position and fixed on the branch; and S4. after the upper end of the ring peeling is fully rooted, the branch is pruned and transplanted. In step S3, 0.75-1.5% of a fungicide is added to the layering propagation matrix, the fungicide is prepared by using a ternary compound of benzene ether carbendazim, oxime ether fungicide and zinc pyrithione as active ingredients, and is supplemented with a surfactant and a solvent. The propagation method can effectively prevent the influence of root rot pathogenic bacteria on the rooting of the branch, is beneficial to the rooting of the high-branch layering, and can further guarantee the survival rate and the propagation efficiency of the high-branch layering, and is beneficial to the smooth development of the seedling raising work of Artocarpus heterophyllus.

The invention discloses a self-cleaning wash-free fabric and a preparation method thereof, and relates to the technical field of fabrics. According to the invention, malic acid is utilized to connect each fiber, so that impurities are not easy to enter the fabric, and then malic acid reacts with maleic anhydride and sodium hydrogen sulfite, so that a sulfonic acid group-metal ion bond is formed on a side chain, the antistatic performance is improved, and the fabric is prevented from being stained with dust; the preparation method comprises the following steps: firstly, preparing a modified cotton fabric, then reacting the modified cotton fabric with 2-hydroxylauric acid, R-aminoethyl-B-aminopropyl trimethoxy silane, perfluorooctyltrimethoxy silane and hexamethyldisiloxane, and polymerizing to obtain the modified cotton fabric which has good waterproof and oil-proof properties; 3-amino-4-nitrobenzaldehyde and 3, 4-diamino propiophenone are utilized to form a benzotriazole group, the anti-ultraviolet effect of the fabric is effectively improved, the benzotriazole group, hydroxylamine hydrochloride and 2-bromoethanol generate an oxime ether compound, the growth of bacteria of the fabric is inhibited, epoxy resin is modified and then coated on the surface of the modified cotton fabric, the epoxy resin and the modified cotton fabric are combined through chemical bonds, and the anti-ultraviolet effect of the fabric is improved. The antibacterial property of the fabric is effectively improved.

The invention relates to the technical field of antibacterial drugs, and particularly discloses a pleuromutilin derivative and application thereof, and the pleuromutilin derivative is structurally characterized in that flavanone or an oximido / oxime ether derivative of flavanone is connected to a side chain of pleuromutilin C14 through mercaptoethylamine, piperazine or an oxygen atom. According to the invention, pleuromutilin is taken as a raw material, flavanone (naringenin and hesperetin) with an antibacterial effect and an oximido / oxime ether derivative thereof are introduced into a pleuromutilin C14 side chain, and the flavanone and the oximido / oxime ether derivative thereof show huge potential as a dominant structural unit due to a specific C6-C3-C6 basic skeleton (C2 and C3 sites are single bonds) and wide antibacterial activity; the flavonoid compound is combined with pleuromutilin to synthesize a plurality of dihydroflavonoid pleuromutilin derivatives with excellent antibacterial activity, and a new choice is provided for designing a new generation of pleuromutilin derivatives through a hybridization strategy, improving the drug characteristics of the pleuromutilin derivatives while improving the activity and anti-infection drugs of the pleuromutilin derivatives.

This invention discloses a chiral amination synthesis process for a pharmaceutical intermediate, comprising two steps: First, hydroxylamine hydrochloride and compound I are mixed in a 40-50 wt% aqueous ethanol solution, and an alkaline reagent is added to adjust the pH to 4-6. The mixture is then heated under reflux to generate an oxime ether compound II. Second, compound II is dissolved in THF or toluene, and a chiral spiroboroate catalyst derived from diphenylvaline is added. A BH3·THF reducing agent is then slowly added dropwise at room temperature to perform an asymmetric reduction to obtain a chiral primary amine compound III. The advantages of this invention are: the reaction route avoids high-risk reagents and harsh conditions, significantly improving process safety; and through process route optimization, efficient asymmetric reduction is achieved, resulting in a product with high chiral purity. The reaction route of this invention features mild reaction conditions, simple operation, and is easy to scale up industrially. The overall route is concise, with short steps and high yield, making it suitable for large-scale industrial production.

This invention proposes a method for preparing chiral α-hydroxy-mercapto-oxime ethers, belonging to the field of organic synthesis technology. The method comprises: S1. protecting the hydroxyl group of chiral α-hydroxypropionamide with a protecting group; S2. reacting the chiral α-protecting group-propionamide sequentially with an oxonium salt donor and an alkoxyamine hydrochloride to obtain chiral 1-[(E)-alkoxynitro]-α-protecting-propyl-1-amine; S3. removing the protecting group from the chiral 1-[(E)-alkoxynitro]-α-protecting-propyl-1-amine to obtain the product. This invention aims to overcome the core defects of existing processes, such as low yield, high impurity content, high reagent safety and environmental risks, high pyridine consumption, and cumbersome operation, and to develop a new process for synthesizing chiral α-hydroxy-mercapto-oxime ethers with high yield, high purity, low cost, high safety, and suitability for industrial scale-up.

The invention relates to a preparation method of a cefixime intermediate, which belongs to the technical field of drug intermediate synthesis, and comprises the following steps: 1, synthesizing an oxime ether intermediate by using tert-butyl acetoacetate as an initial raw material and using a two-step one-pot method; in the second step, a chlorination-cyclization one-pot reaction is adopted, wherein the oxime ether intermediate reacts with NOCl generated by hydrochloric acid and tert-butyl nitrite, and a chlorination product is generated; carrying out cyclization reaction with thiourea and triethylamine to obtain an acid intermediate; and 3, in order to avoid decomposition of the product, respectively pulping the acid intermediates-dichloromethane, DM-triethylamine and triphenylphosphine-dichloromethane, and mixing and reacting in the microchannel to finally obtain the cefixime intermediate. The whole synthesis route avoids strong acid and other raw materials with great environmental pollution, avoids generation of byproducts, obtains high-yield and high-purity products, and shows better economic advantages.

The invention belongs to the technical field of organic synthesis, and discloses a preparation method of oxime ether and methoxyamine hydrochloride. According to the method, tert-butyl alcohol is used as a solvent, a methylation reagent, sodium hydroxide, ketoxime and the solvent are subjected to a condensation reaction, reaction liquid is subjected to rectification separation, fractions are collected, and oxime ether is obtained; and mixing the tower bottom residual liquid with a hydrochloric acid solution, and carrying out hydrolysis reaction to obtain methoxyamine hydrochloride. Efficient dissolution of a methylation reagent is achieved through a tert-butyl alcohol solvent system, an oxime ether intermediate is prepared in cooperation with a low-temperature condensation reaction, a hydrochloric acid hydrolysis reaction is completed in a tower after rectification separation, and finally methoxyamine hydrochloride and sodium chloride are obtained. And through solvent innovation, process integration and premixing control technologies, the reaction selectivity is remarkably improved, and the raw material consumption is reduced.

The invention belongs to the technical field of chemical pharmacy, and particularly relates to a method for preparing a trifloxystrobin intermediate through Taylor flow reinforced oxime ether photobromination. The method comprises the following steps: S1, introducing an organic phase containing oxime ether and bromine and a second phase immiscible with the organic phase into a continuous flow photochemical microchannel reactor; and S2, enabling the organic phase containing oxime ether and bromine and a second phase immiscible with the organic phase to form a Taylor flow under the irradiation of ultraviolet light, and carrying out a reaction to prepare the oxime ether bromide. According to the method, the reaction efficiency is remarkably improved through a Taylor flow system, the product yield is improved while the reaction time is shortened, side reactions are effectively inhibited, and an efficient and high-purity solution is provided for production of the trifloxystrobin intermediate.

This invention relates to the synthesis and application of indole-3-lactone analogs with oxime ether linkages. The general formula for this class of compounds is shown in (I), where R1 is methyl, ethyl, n-propyl, n-butyl, n-pentyl, isopropyl, isobutyl, phenyl, or benzyl. Starting with indigo as a raw material, the product is obtained through nucleophilic substitution, Wolff-Kishner-Huang Minglong reduction reaction, and Williamson ether synthesis reaction. Using *Trichosanthes kirilowii* seeds (… O. aegyptiaca As a target for control, this series of compounds were applied to test seed germination activity. These compounds exhibited good seed germination activity and can be applied to the seed germination of the parasitic weed *Orobanche deserticola*, for the development of a "suicidal" herbicide for *Orobanche deserticola*. This invention also includes its use in combination with agriculturally acceptable adjuvants, synergists, or commercial herbicides to prevent diseases caused by parasitic weeds such as *Orobanche deserticola* or *Orobanche spp.*.

The disclosure relates to 1-(bicyclo[2.2.1]hept-5-en-2-yl)ethan-1-one O-methyl oxime possessing powerful green fruity anisic banana olfactory properties. The invention furthermore refers to fragrance compositions comprising it and to a method of improving, enhancing or modifying a consumer base product by incorporating it into said product.

The invention discloses a pesticide composition which contains a cyclohexenedione lactic acid oxime ether compound as shown in a formula I, a stereoisomer, a tautomer, a solvate or a pesticide acceptable salt thereof and a herbicide B. The definitions of R1-R4 and the herbicide B are as defined in the specification. The composition disclosed by the invention has a relatively good weeding effect and a relatively good application prospect.

The invention discloses an application of a lignite residue as a catalyst for catalytic synthesis of an oxime ether acetate compound and a preparation method of the oxime ether acetate compound. The method comprises the following steps: taking oximes and aryl diazonium ester compounds as raw materials, and taking the lignite residue (Zhaotong, Yunnan) as the catalyst. The lignite residue catalyst is wide in source, low in cost and easy to obtain, mild in reaction condition, wide in substrate application range, good in yield and capable of achieving gram-scale reaction and has industrial application prospects. Meanwhile, waste resources can be recycled, the problem that the lignite residues are difficult to treat is solved, and the purposes of environmental protection and green chemistry are met.