17 results about "Methoxamine" patented technology

The invention belongs to the technical field of organic synthetic chemistry and pesticide science, and particularly relates to an indole-containing amide derivative as well as a preparation method and application thereof, and the indole-containing amide derivative has a structure as shown in a formula I or a formula II, through an active substructure splicing strategy, indole is used as a parent skeleton, amido bonds are ingeniously introduced for structural diversity optimization and modification, active functional groups such as methoxyamine are further introduced, and a series of indole amide derivatives with novel structures are designed and synthesized. Through determination, the screened series of compounds show good antibacterial activity, and a plurality of compounds show excellent prevention and treatment effects on various important crop diseases.

The present invention relates to a synthetic method of 2-methyl-α-methoxyiminophenylacetic acid methyl ester, and the method flow comprises the following: Step 1: using o-methylphenylacetic acid or o-methylphenylacetamide or o-methylphenylacetic acid methyl ester as raw material, first directly oximating and esterifying with sodium nitrite in sulfuric acid in a solvent; Step 2: "one-pot method" hydrogenation of sodium hydroxide or potassium hydroxide to control pH value, and reacting with dimethyl sulfate to obtain 2-methyl-α-methoxyiminophenylacetic acid methyl ester. The present invention uses o-methylphenylacetic acid or o-methylphenylacetamide or o-methylphenylacetic acid methyl ester as raw material, and adopts safe and reliable sodium nitrite as oximation reagent, avoids using nitrite esters that are flammable and explosive, avoids using expensive methoxyamine hydrochloride, has safe and reliable reaction, low raw material cost, and adopts "one-pot method" in the operation process, has simple and smooth process, mild reaction conditions, and is suitable for industrialized amplification production.

The invention relates to the field of organic synthesis, in particular to a preparation method of 1, 2, 3-benzotriazine-4-ketone, which comprises the following steps: S1, under the catalytic action of a condensing agent T3P, directly carrying out amidation reaction on anthranilic acid and methoxyamine hydrochloride to obtain 2-amino-N-methoxybenzamide; s2, under the condition of a diazotization reaction, the 2-amino-N-methoxybenzamide is converted into 3-methoxy-1, 2, 3-benzotriazine-4-ketone, and the 3-methoxy-1, 2, 3-benzotriazine-4-ketone is converted into 2-methoxy-1, 2, 3-benzotriazine-4-ketone; and S3, reducing the 3-methoxy-1, 2, 3-benzotriazine-4-ketone into the 1, 2, 3-benzotriazine-4-ketone under the condition of palladium on carbon / hydrogen gas, so as to obtain the 1, 2, 3-benzotriazine-4-ketone. The preparation method provided by the invention has the advantages of easily available raw materials, easily separated products and high yield, and is suitable for industrial production.

The utility model relates to a mother liquor recycling device for producing methoxyamine hydrochloride, which comprises a recycling tank and an outer cooling interlayer, and is technically characterized in that a central cooling vertical pipe is supported in the recycling tank by a bearing, and the upper end and the lower end of the central cooling vertical pipe are connected with a second cooling medium outlet and a second cooling medium inlet by an upper rotary joint and a lower rotary joint; an annular scraping assembly is arranged between the recycling tank and the central cooling vertical pipe, the annular scraping assembly is composed of an outer scraping ring, an inner scraping ring, an annular hollowed-out plate connected between the upper edges of the inner scraping ring and the outer scraping ring and a filter screen layer arranged on the annular hollowed-out plate, an electric push rod is fixed to the top face of the recycling tank, and the lower end of a telescopic rod is fixedly connected with the annular hollowed-out plate; a discharging scraper is arranged on the lower portion of the central cooling vertical pipe, a crystal material discharging port is formed in the bottom face of the recycling tank, a liquid outlet is formed in the lower portion of the side wall of the recycling tank, a circulating inlet is formed in the upper portion of the side wall of the recycling tank, the liquid outlet is provided with a circulating branch communicated with the circulating inlet, and a circulating pump is arranged on the circulating branch. The device further improves the recovery efficiency.

The invention discloses a preparation method for preparing methoxyamine hydrochloride by using 2, 3-butanedione, which comprises the following steps: S1, adding 2, 3-butanedione and hydroxylamine hydrochloride into water, and carrying out oximation reaction under the action of alkali to prepare 2, 3-butanedioxime; s2, 2, 3-dimethylglyoxime and dimethyl sulfate are subjected to a methylation reaction, 2, 3-bis (methoxyimino) butane is prepared, and in the reaction process, alkali liquor is adopted to control the pH of a reaction system to be 7-9; s3, the 2, 3-bis (methoxyimino) butane is subjected to an acidolysis reaction, and methoxyamine hydrochloride is prepared. According to the method, 2, 3-butanedione and hydroxylamine hydrochloride are taken as raw materials, so that the conversion rate of methylation reaction is increased, the generation of polymethylation impurities (O, N-dimethyl hydroxylamine hydrochloride) is reduced, the yield is relatively high, meanwhile, the reaction condition is mild, the operation is simple, synthesis is easy, the byproduct 2, 3-butanedione can be recycled, the material utilization rate is high, and the method is suitable for industrial production. And the cost and the energy consumption can be reduced.

The invention discloses a mother liquor tail gas heat recovery device and method in methoxyamine production. The mother liquor tail gas heat recovery device comprises a mother liquor kettle, a waste heat exchanger, an efficient gas-liquid separation tank, a liquid caustic soda temporary storage tank, a liquid caustic soda circulating pump and a distillation kettle, an outlet of the mother liquor kettle is communicated with a gas phase inlet of the waste heat exchanger through a pipeline, a gas phase outlet of the waste heat exchanger is communicated with an inlet of the efficient gas-liquid separation tank through a pipeline, and a gas phase outlet of the efficient gas-liquid separation tank is connected into a tail gas system through a pipeline. According to the process, heat in the mother liquor tail gas can be recycled to the maximum extent, the initial temperature of fed caustic soda liquid can be effectively increased, the amount of steam used in the heating process in the earlier stage of methoxyamine distillation is reduced, a low-temperature gas phase at an outlet of the waste heat exchanger enters the efficient gas-liquid separation tank, liquid drops entrained in the low-temperature gas phase can be effectively recycled, and the quality of the methoxyamine is improved. And meanwhile, the tail gas subjected to efficient separation is relatively modified, so that subsequent further treatment on the tail gas is facilitated.

The invention provides a four-step synthesis method of rerugolix, and belongs to the technical field of medicine synthesis. The four-step synthesis comprises the following steps: (1) reacting a compound G with 3-amino-6-methoxypyridazine under the action of a condensing agent and alkali to obtain a compound H; (2) carrying out cyclization reaction on the compound H under the action of alkali to obtain a compound I; (3) obtaining a compound J from the compound I and carbamic acid ester under the action of metal palladium or copper, a ligand and alkali; and (4) carrying out amine ester exchange reaction on the compound J and methoxyamine hydrochloride under the action of alkali to obtain the rerugolix. The method has the advantages of mild reaction conditions, simplicity and convenience in operation, high reaction yield, safer process, easiness in product purification, low production cost, greenness, environmental friendliness and suitability for commercial scale.

The present invention provides a preparation method of (Z)-α-(methoxyimino)furan-2-acetic acid, which belongs to the field of pharmaceutical intermediates. Furfural and methoxyamine hydrochloride are condensed under an acid binding agent to obtain 2-furaldehyde O-methyloxime, followed by addition with a cyanating agent in DMSO to obtain 2-(furan-2-yl)-2-(methoxyamino)acetonitrile, which is then oxidized with ferric chloride to obtain (Z)-N-methoxyfuran-2-imido cyanide, and finally hydrolyzed with sulfuric acid solution to obtain (Z)-α-(methoxyimino)furan-2-acetic acid. The preparation method of the present invention has the advantages of continuous operation between steps, high yield, purity of more than 99%, and avoids the problems of purification difficulty and color caused by configuration.

A process (100) and reactor assembly (200) for synthesis of methoxylamine hydrochloride (MAHCl) is disclosed. Methoxylamine hydrochloride is a key reagent for the preparation of one or more than one oxime derivative. The present disclosure relates to development of a process (100) for preparation of methoxylamine hydrochloride product by utilizing different reaction routes which minimizes the time consumption and is an economical process thereby minimizing the energy consumption of the overall process.

The invention provides a high performance liquid chromatography quantitative analysis method of methoxyamine hydrochloride, which comprises the following steps: preparation of solutions: preparation of reference solutions with a series of concentration gradients: weighing methoxyamine hydrochloride standard substances according to different concentrations respectively, adding a sodium hydroxide solution for dissolving, then adding an organic solvent, and fixing the volume; preparing a test solution, namely weighing a test sample, neutralizing the test sample to a specific pH value by using a sodium hydroxide solution, then adding an organic solvent, and fixing the volume; high performance liquid chromatography is adopted for quantitative detection, and quantitative analysis is carried out according to a linear regression curve; wherein the mobile phase is deionized water, and the mobile phase B is chromatographic methanol. Compared with traditional acid-base titration method quantification and potentiometric titration method quantification, the method provided by the invention has the advantages that the result accuracy is not interfered by the main impurities ammonium chloride and N, O-dimethylhydroxylamine hydrochloride in the methoxylamine hydrochloride finished product, the sensitivity is higher, and the accuracy is higher. The method has important practical significance in the quality control aspect of industrial production of methoxyamine hydrochloride.

The invention provides a method for preparing dimethyl hydroxylamine hydrochloride from waste liquid generated during production of methoxylamine hydrochloride, and relates to the technical field of advanced environmental protection, which comprises the following steps: adding alkali into the waste liquid generated during production of methoxylamine hydrochloride to dissociate methoxylamine hydrochloride and dimethyl hydroxylamine hydrochloride, and then adding an acylation reagent for acylation; adding a methylation reagent for methylation; finally, adding acid for hydrolysis, cooling, dissociating with sodium hydroxide, and distilling to obtain a dimethyl hydroxylamine aqueous solution at 80-90 DEG C; and finally, 37% hydrochloric acid is added into the fraction for salifying, then vacuum concentration is performed, methanol is added into the obtained solid for recrystallization to obtain the dimethylhydroxylamine hydrochloride, resources are recycled, mother liquor generated in industrial production of methoxylamine hydrochloride can be reused, waste of the resources is avoided, and the production cost is reduced. The method comprises the steps of heating reflux hydrolysis, distillation, salification, recrystallization and the like, so that impurities can be effectively removed, and the purity of the dimethylhydroxylamine hydrochloride is improved. And heating reflux hydrolysis is performed for 2-3 hours, so that the reaction is relatively sufficient, and the quality of the subsequently obtained product is higher.

The present invention belongs to the technical field of organic complex synthesis, and specifically relates to a metal complex and its preparation method and application. The general formula of the metal complex is L-M, wherein L is a ligand, M is a metal salt, and the ligand is benzylquinine-3-ketoxime or benzylquinine-3-ketone-O-methyloxime ether. The benzylquinine-3-ketoxime is prepared from an ethanol solution containing ketone, hydroxylamine hydrochloride and anhydrous potassium carbonate; the benzylquinine-3-ketone-O-methyloxime ether is prepared from an ethanol solution containing ketone, methoxyamine hydrochloride and anhydrous potassium carbonate. The preparation method of the metal complex is to add an aqueous solution containing a metal salt dropwise to a methanol solution containing a ligand, carry out a coordination reaction, and filter to obtain a target product. The preparation method has the advantages of simple process, mild conditions, low cost, and easy industrialization. The metal complex provided by the present invention can be used to prepare an antibacterial agent, which has the advantages of high efficiency, low toxicity and environmental protection.

The application relates to a one-pot method for synthesizing an intermediate oxime ether of a bactericide, and belongs to the technical field of organic synthesis. The method flow comprises the following steps: Step 1: adding o-halotoluene, methyl glyoxylate, methoxyamine hydrochloride and a solvent into a reaction bottle, wherein X in the o-halotoluene is chlorine, adding a base and a catalyst, the catalyst is Cu-TMEDA, and the reaction is carried out after heat preservation; Step 2: after the reaction is completed, water is added for washing, and the organic phase is concentrated under reduced pressure to recover the solvent to obtain the oxime ether. In the application, compared with a traditional oxime ether synthesis method, the oxime ether is synthesized by using o-halotoluene, methyl glyoxylate and methoxyamine hydrochloride as raw materials in a one-pot catalytic synthesis mode, the reaction process is safe and reliable, the raw material cost is low, and the three-waste output is less. The oxime ether synthesis method is simple and efficient, the reaction condition is mild, a toxic sodium cyanide reagent or flammable and explosive tert-butyl nitrite is not needed, the reaction process is safer, and the method is suitable for industrialized scale production.

The invention discloses a preparation method of (E)-(5, 6-dihydro-[1, 4, 2]-dioxazine-3-yl)-(2-hydroxyphenyl)-ketone-O-methyl oxime, which comprises the following steps: (1) in the presence of inorganic alkali, carrying out amination reaction on 2-hydroxy-2 '-nitroacetophenone and methoxyamine hydrochloride to obtain 1-(2-hydroxyphenyl)-2-nitro-ethanone-O-methyl oxime; (2) heating the reaction system, and carrying out high-temperature cyclization, so as to obtain benzofuran-2, 3-diketone-3-(O-methyl oxime)-2-oxime; (3) supplementing inorganic alkali into the reaction system, and then adding 2-chloroethanol to carry out substitution reaction, so as to obtain benzofuran-2, 3-diketone-2-[O-(2-ethoxyl) oxime]-3-(O-methyl oxime); and (4) supplementing inorganic alkali into the reaction system, then heating to carry out high-temperature cyclization and alkaline rearrangement, and finally carrying out post-treatment to obtain the (E)-(5, 6-dihydro-[1, 4, 2]-dioxazine-3-yl)-(2-hydroxyphenyl)-ketone-O-methyl oxime. The four-step reaction yield can reach about 40%, the product purity can reach 96% or above, the quality is obviously high, and meanwhile the method is low in production cost, mild in reaction condition, simple and convenient in technological operation and suitable for large-scale industrial production.

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 application discloses a method for cleaning the surface pollution of a polyamide composite membrane and simultaneously repairing the water flux and salt retention rate of the polyamide composite membrane, and the method comprises the following steps: step 1, under normal temperature conditions, immersing a polyamide composite membrane damaged by oxidation of active chlorine substances into a repairing solution, wherein the repairing solution is composed of a methoxyamine salt and a metal catalyst; the methoxyamine salt is one or a combination of two or more of methoxyamine hydrochloride, methoxyamine sulfate, methoxyamine phosphate, methoxyamine acetate, methoxyamine trifluoroacetate, methoxyamine formate, methoxyamine methanesulfonate, methoxyamine trifluoromethanesulfonate and methoxyamine p-toluenesulfonate; and step 2, after 2-5 hours of repairing, taking out the polyamide composite membrane and washing away the residual repairing solution with water. The method can clean and remove the inorganic scaling, organic matter and other pollutants on the surface of the polyamide composite membrane while repairing the water flux and salt retention rate of the polyamide membrane damaged by sodium hypochlorite oxidation.

The application discloses a mother liquor tail gas heat recovery device and method in methoxyamine production, which comprises a mother liquor kettle, a waste heat exchanger, a high-efficiency gas-liquid separation tank, a liquid alkali temporary storage tank, a liquid alkali circulating pump and a distillation kettle; the outlet of the mother liquor kettle is communicated with the gas phase inlet of the waste heat exchanger through a pipeline, the gas phase outlet of the waste heat exchanger is communicated with the inlet of the high-efficiency gas-liquid separation tank through a pipeline, and the gas phase outlet of the high-efficiency gas-liquid separation tank is connected to a tail gas system through a pipeline. The process can maximize the recovery of the heat in the mother liquor tail gas, effectively improve the initial temperature of the feeding liquid alkali, reduce the steam consumption in the early warming process of methoxyamine distillation, and enable the low-temperature gas phase at the outlet of the waste heat exchanger to enter the high-efficiency gas-liquid separation tank, so that the liquid drops entrained in the low-temperature gas phase can be effectively recovered; meanwhile, the tail gas after high-efficiency separation is relatively modified, and the subsequent further treatment of the tail gas is facilitated.