19 results about "Acetanilide" patented technology

The invention discloses a preparation method of N-methyl o-fluoroaniline, which is characterized in that o-fluoroaniline is used as a starting raw material, and a target product is efficiently synthesized through three steps of reaction: step 1, in the presence of a solvent and alkali, o-fluoroaniline and acetyl chloride are acetylated at low temperature to generate 2-fluoro-acetanilide, and the product is directly used for the next step after being roughly purified; 2, under the action of a solvent and alkali, carrying out controllable methylation on the 2-fluorine-acetanilide and dimethyl carbonate to obtain 2-fluorine-N-methylacetanilide; and 3, removing acetyl protection through acidic hydrolysis, and adding sodium thiosulfate to prevent oxidation to finally obtain a high-purity product. According to the method, excessive methylation is avoided through an acetyl protection strategy, the process does not need high-risk operations such as ultralow temperature and high pressure, the operation is simple and convenient, the energy consumption is low, and the product purity is gt; the total yield reaches 79.86%, and the method is green, safe and suitable for industrial production.

The invention discloses an HRP chemiluminescent substrate system, a kit and a preparation method, the HRP chemiluminescent substrate system is composed of a liquid A and a liquid B which are physically isolated and stored; the solution A is an alkaline buffer system with the pH value of 9.0-9.6, and comprises isoluminol or a salt substrate thereof, a cationic surface active agent CTAC and a metal chelating agent diethylene triamine pentaacetic acid; and the solution B is an acidic solution with the pH value of 4.5-5.5, and comprises an oxidizing agent and a reinforcing agent N-(3-chloro-4-hydroxyphenyl) acetanilide. According to the invention, the reinforcing agent N-(3-chloro-4-hydroxyphenyl) acetanilide is placed in the acidic liquid B, when the acidic liquid B is mixed with the alkaline liquid A, the mixed system is maintained at a specific pH value of 8.3-8.6, and the reinforcing agent is rapidly dissociated into phenoxy anions; and carrying out in-situ capture and enrichment on a micelle interface by CTAC cationic micelles with positive charges, which exist in the solution A in advance, through electrostatic attraction. And in cooperation with a low-ion-strength environment brought by no buffer salt in the liquid B, the system ensures the high activity of the HRP enzyme, realizes directional interface catalysis of the enhancer, and significantly improves the luminous efficiency and stability.

The invention relates to the field of pesticide synthesis, in particular to a synthesis method of ethonicotinic acid. 5-ethyl pyridine-2. 3-dicarboxylic acid diethyl ester and 2-amino-2. 3-dimethyl butyramide are used as raw materials and react in a sodium ethoxide ethanol solution at the temperature of 50-70 DEG C, hydrogen chloride gas is introduced into a system for acidification after the reaction is completed, and imazethapyr and a by-product sodium chloride are obtained. The hydrogen chloride gas is directly introduced in the acidification process, and the acidification process is free of hydration, so that on one hand, no direct wastewater is generated, the generation of wastewater with high salt content and high organic matter content is avoided, the treatment cost is reduced, on the other hand, the byproduct sodium chloride is firstly removed from the system by controlling the ethanol amount of the system, and then concentration and crystallization are performed; the high-purity imazethapyr of which the purity is greater than 99% is obtained by utilizing the solubility of the solvent ethanol to impurities, and the quality of both byproducts and main products is at a higher level in the industry.

Herbicide concentrate compositions containing a combination of herbicides are provided; in particular, the present invention relates to aqueous herbicide concentrate compositions containing a particulate encapsulated acetanilide herbicide and a protoporphyrinogen oxidase inhibitor (PPO inhibitor).

The invention provides a phosphotungstic acid supported Zr-SBA-12 molecular sieve as well as a preparation method and application thereof, and belongs to the technical field of molecular sieve catalysts. According to the preparation method, an SBA-12 molecular sieve is taken as a carrier, Zr is introduced into an SBA-12 molecular sieve framework through a hydrothermal synthesis method, then phosphotungstic acid is loaded on the Zr-SBA-12 molecular sieve through a direct hydrothermal method, and the composite catalyst with high acidity, site density and good structural stability is obtained. Through the synergistic effect of the metal Zr and the phosphotungstic acid, the number of acid sites and the catalytic activity of the catalyst are remarkably improved, the surface acidity of the molecular sieve is improved, and the problems of difficult recovery and high cost are solved. And the phosphotungstic acid supported Zr-SBA-12 molecular sieve as a catalyst has important research value and application prospect in the field of acetanilide nitration reaction.

The application belongs to the technical field of organic synthesis, and particularly relates to a preparation method of 4-amino-2-methylbenzoic acid, and more particularly relates to a preparation method of 4-amino-2-methylbenzoic acid as a raw material of a tolvaptan intermediate, wherein 3-methylaniline is used as a raw material to prepare 3-methylacetanilide with an acylating agent, the 3-methylacetanilide is subjected to Friedel-Crafts acylation with oxalyl chloride under a Lewis acid catalytic system to prepare 4-acetylamino-2-methylbenzoic acid, and finally, the 4-acetylamino-2-methylbenzoic acid is deprotected under alkaline conditions, and then acidified to obtain the target compound 4-amino-2-methylbenzoic acid, wherein the raw material used in the preparation method is cheap and easy to obtain, the production equipment has low requirements, the process condition is simple, the safety factor is high, no ammonia nitrogen and other three wastes are generated, the cost is low, and the industrialized production is easy to implement.

The invention discloses a synthesis method of an atorvastatin intermediate. The method comprises the following steps of: catalyzing alpha-chlorophenylacetyl chloride and fluorobenzene to perform Friedel-Crafts acylation reaction by taking immobilized Bronsted-Lewis acidic ionic liquid as a catalyst, and performing condensation reaction on a product and isobutyryl acetanilide under the action of alkali and the assistance of microwaves, the preparation method comprises the following steps: adding 2-[2-(4-fluorophenyl)-2-oxo-1-phenylethyl]-4-methyl-3-oxo-N-phenyl pentanamide into an organic solvent to obtain the atorvastatin intermediate 2-[2-(4-fluorophenyl)-2-oxo-1- By utilizing the characteristics of large specific surface area and abundant active sites of graphite-like carbon nitride, the graphite-like carbon nitride is used as an ionic liquid immobilization carrier and a parent nucleus to participate in the ionic liquid preparation process, the catalytic activity of the ionic liquid is retained, the catalyst is simple to separate, the reaction rate and selectivity are improved, the steps are simple, and the method is suitable for industrial production. The method has the advantages of mild reaction conditions in each step, low cost, high yield and easily available reaction conditions, and improves the application prospect.

1-methyl-2-carboxyl-3-acetanilide indole compounds and applications thereof. The compounds can block the interaction between NLRP3 and NEK7, effectively inhibit the activation and assembly of NLRP3 inflammasome, and have good prevention and treatment effect on NLRP3 inflammasome related inflammatory diseases such as Alzheimer's disease and Parkinson's disease. Thus, the compounds can be used for preparing drugs for treating and / or preventing NLRP3 inflammasome related inflammatory diseases, and provide a new choice for the development of NLRP3 inflammasome small molecule inhibitors.

The application discloses a synthesis method of an atorvastatin intermediate. The method comprises the following steps: firstly, using a solidized Brønsted-Lewis acidic ionic liquid as a catalyst, catalyzing a Friedel-Crafts acylation reaction of alpha-chlorobenzene acyl chloride and fluorobenzene, then, under the action of alkali and microwave assistance, performing a condensation reaction of the product and isobutyryl acetanilide, and finally, obtaining the atorvastatin intermediate 2-[2-(4-fluorophenyl)-2-oxo-1-phenylethyl]-4-methyl-3-oxo-N-phenylpentanamide. The method uses the characteristics of a large specific surface area and rich active sites of graphite-like carbon nitride, simultaneously uses the graphite-like carbon nitride as an ionic liquid solid carrier and as a mother nucleus to participate in the preparation process of the ionic liquid, retains the catalytic activity of the ionic liquid, improves the reaction rate and selectivity through simple separation of the catalyst, and has the advantages of low cost, high yield, easy reaction conditions, and improved application prospect.

The application discloses a continuous separation system and method for liquid aniline derivative intermediates, and the liquid aniline derivative intermediates are liquid 3-(N,N-diallyl) amino-4-methoxy acetanilide or liquid 3-(N,N-diethyl) amino acetanilide. The application can quickly separate product heavy oil, mother liquor water and floating oil components by using a continuous oil-water separator, a floating oil intermediate tank and a product oil intermediate tank. The emulsified materials in the mother liquor water can be effectively recovered by using the mother liquor intermediate tank for salting-out demulsification. The separated mother liquor clear liquid enters an MVR evaporation system, and ammonium chloride salt and distilled water are obtained through evaporation, concentration and crystallization. The ammonium chloride concentrate can be recycled for salting-out demulsification. After the liquid aniline derivative intermediate crude product is subjected to the continuous separation system and method, the separation efficiency of the liquid material is high, the overall material yield is improved, the solid content of the product is obviously improved, the system stability is good, and the wastewater treatment cost is reduced.

The invention discloses a method for recycling o-methyl-bis-acetanilide mother liquor through multistage membrane separation, and belongs to the field of chemical engineering. The method comprises the following steps: firstly, fully stirring the obsolete mother liquor of o-methylacetoacetanilide, then filtering through a molecular sieve filter membrane to remove suspended solids with larger particle sizes, directly treating filter residues in an incinerator, and then pumping filtrate into pervaporation membrane equipment; under the reverse osmosis action of the pervaporation membrane, water molecules are separated through the pervaporation membrane to obtain high-purity water which can be directly reused as reclaimed water; and the residual liquid is directly pumped into the evaporation tower and is condensed and refluxed to obtain high-purity ethanol which can be used as ethanol for preparing mother liquor next time, and the residual liquid at the bottom of the evaporation tower can be directly sent to an incinerator for treatment.

The invention discloses a continuous reaction research process of low-biphenylamine impurity 2, 4-dimethyl-bis-acetanilide, and belongs to the field of chemical synthesis. The invention aims to provide the continuous reaction research process for the low-bis-phenylamine impurity 2, 4-dimethyl-bis-acetanilide (2, 4-dimethyl-N-acetoacetanilide), the retention time of the 2, 4-dimethyl-N-acetoacetanilide raw material is shortened, the bis (2, 4-dimethyl phenyl) amine impurity is reduced, the yield of the 2, 4-dimethyl-N-acetoacetanilide is increased, and the production cost is reduced. Meanwhile, the auto-polymerization of the diketene is reduced, the consumption of the 2, 4-dimethylaniline is reduced, and the problems of high impurity content of the bis (2, 4-dimethylphenyl) amine in the existing 2, 4-dimethyl-N-acetoacetanilide and poor batch stability are solved.

The application provides a kind of catalyst recyclable carboxin synthesis method, belong to organic synthesis technical field, comprising: the condensation reaction of alpha-chloroacetyl acetanilide and 2-mercaptoethanol under alkaline conditions, intermediate is obtained by separation;With toluene as solvent, the obtained intermediate is mixed with ionic liquid catalyst to form a reaction system, heating reaction, after the reaction is completed, the temperature of the reaction system is reduced to 5-25 DEG C, the reaction system is layered, then separation treatment is carried out, carboxin product and separated ionic liquid catalyst are obtained, then the separated ionic liquid catalyst is regenerated by dehydration and recycled;Wherein, the ionic liquid catalyst is 1-(polyethylene glycol monomethyl ether group)-3-(3-sulfopropyl) imidazole hydrogen sulfate salt.The reaction system has homogeneous high-efficiency conversion at high temperature and automatic separation at low temperature, which realizes the green upgrading of carboxin synthesis process.

The invention discloses a preparation method of a fluorescent dye crude product, which is characterized by comprising the following steps: adding 1, 1, 2-trimethyl-3-(4-sulfonic acid butyl)-1H-benzo [e] indole inner salt and 2-[6-(acetanilino)-1, 3, 5-hexantrienyl]-1, 1-dimethyl-3-sulfonic acid butyl-1H-benzo [e] indole inner salt into absolute ethyl alcohol, dropwise adding triethylamine, reacting for 4-5 hours, filtering, washing, and drying to obtain the fluorescent dye crude product, namely the 2-[6-(acetanilino)-1, 3, 5-hexantrienyl]-1, 1-dimethyl-3-sulfonic acid butyl-1H-benzo [e] indole. Dropwise adding an absolute ethyl alcohol solution of sodium iodide, after dropwise adding, adding purified water, heating and stirring to completely dissolve the solid, and then cooling and crystallizing to obtain a fluorescent dye crude product; meanwhile, the invention discloses a refining method of the fluorescent dye crude product. And the yield of the fluorescent dye is ensured, and impurities and solvent residues meet the limit.

This invention relates to a method for the selective nitration of 4-acetamidoanisole using a continuous flow microchannel reactor, belonging to the field of compound synthesis. The method includes: mixing 4-acetamidoanisole with a solvent to obtain feed solution A; using nitric acid as feed solution B; washing the microchannel reaction system with a solvent; pumping feed solution A and feed solution B separately into the microchannel reactor using metering pumps; after the reaction is complete, the product flows out from the outlet of the microchannel reactor, and the reaction solution is collected; diluting the reaction solution with ice water, precipitating the product, filtering, washing, and drying to obtain 4-acetamido-2-nitroanisole, or separating the reaction solution by washing with water, distilling under reduced pressure, and drying to obtain 4-methoxy-2-nitroacetanilide. This method only requires changing the solvent system of one feed solution to obtain two isomers with excellent selectivity. It features high reaction safety, short reaction time, simple post-processing, avoids the dangers of batch nitration reactions, and significantly reduces economic costs.

The invention relates to the technical field of pharmaceutical analysis, in particular to a method for detecting bromoacetoacetanilide and aniline in a rebamipide tablet, impurities are detected by using a liquid chromatography-mass spectrometry technology, adopting an Agilent C18 chromatographic column and taking a 0.1% formic acid solution-acetonitrile mixed solution as a mobile phase, and the content of the impurities is calculated by adopting an external standard method. According to the method for detecting bromoacetoacetanilide and aniline in the rebamipide tablet, a liquid chromatography-mass spectrometry technology is adopted, quantitative detection of bromoacetoacetanilide and aniline is achieved, and the method is high in specificity, high in sensitivity, good in stability, high in sensitivity, high in sensitivity and high in reliability. According to the method, the content of bromoacetoacetanilide and aniline in the rebamipide tablet can be effectively measured, the quality control of the rebamipide tablet is perfected, the product quality is controllable, and the safety and effectiveness of the product are ensured.

The present application relates to the technical field of organic synthesis, and particularly relates to an environment-friendly synthesis method of 6-chloro-2-hydroxyquinolin. The specific scheme is that p-chloro-o-nitroacetacetanilide is closed under the action of a certain concentration of liquid alkali, electrolytic reduction is used instead of traditional reductant reduction to prepare a sodium salt, and the sodium salt is subjected to acidification treatment to obtain a pyridyl-quinoline intermediate (6-chloro-2-hydroxyquinolin). The method greatly reduces the discharge of sulfur-containing wastewater, has mild reaction conditions, short reaction period, protects the environment, and reduces the cost of synthesizing the pyridyl-quinoline intermediate (6-chloro-2-hydroxyquinolin).

The invention discloses a 2-(indole-3-yl)-2-oxo acetanilide compound and a medical application of the 2-(indole-3-yl)-2-oxo acetanilide compound. The structure of the 2-(indole-3-yl)-2-oxoacetanilide derivative is shown as a formula I or pharmaceutically acceptable salt thereof, R1 is hydrogen, C1-C4 straight chain or branched chain alkyl, R2 is substituted or unsubstituted pyridyl, the substituent group of the pyridyl is halogen, C1-C4 straight chain or branched chain alkyl, and R3 is hydrogen or halogen, and the structural formula of the 2-(indole-3-yl)-2-oxoacetanilide derivative is shown as a formula I. The invention further discloses a preparation method of the 2-(indole-3-yl)-2-oxoacetanilide derivative. The compound provided by the invention can be used for treating diseases related to tubulin polymerization. The invention further discloses application of the 2-(indole-3-yl)-2-oxoacetanilide derivative or the pharmaceutically acceptable salt of the 2-(indole-3-yl)-2-oxoacetanilide derivative in preparation of a tubulin polymerization inhibitor. The invention further discloses application of the 2-(indol-3-yl)-2-oxoacetanilide derivative or the pharmaceutically acceptable salt of the 2-(indol-3-yl)-2-oxoacetanilide derivative to preparation of a medicine for treating diseases related to tubulin polymerization.

A standard solution for basic nitrogen in a simulated oil product comprises acetanilide and the simulated oil product, the simulated oil product is composed of n-hexadecane, n-undecane, cyclopentane and isooctane according to the mass ratio of 1: (1.5-2.5): (2.5-3.5): (3.5-4.5), and the purity of the acetanilide is higher than 99 wt%, more preferably higher than 99.5%; the concentration of acetanilide in the standard solution is 0.1-1g / L. N-hexadecane, n-undecane, cyclopentane and isooctane in a specific ratio are used as solvents, the molecular structure is closer to that of light fuel oil, the selected components are stable in chemical property, and the chemical stability of a standard solution can be guaranteed; acetanilide has typical characteristics of organic nitrogen compounds in oil products, and when acetanilide is used as a representative of organic nitrogen, the acetanilide is single in source and stable in chemical property; the purifying agent is used for removing trace unsaturated hydrocarbon in the simulated oil product, and polymerization of the unsaturated hydrocarbon in the long-term storage process can be eliminated. The acetanilide concentration change amplitude of the obtained standard substance solution within one year is less than 1%.