175 results about "Acetyl chloride" patented technology

The invention discloses piperonyl butoxide and a preparation method thereof. The preparation method comprises the following steps: carrying out mixing reaction on dihydrosassafras oil, acetyl chloride and trioxymethylene in the presence of concentrated hydrochloric acid; after the reaction is finished, chloromethyl material reaction liquid is obtained; mixing and reacting the chloromethyl material reaction liquid with sodium hydroxide and diethylene glycol monobutyl ether to obtain a product containing piperonyl butoxide. According to the preparation method of piperonyl butoxide, the dihydrosassafras oil, acetyl chloride and trioxymethylene are subjected to chloromethylation reaction in the presence of a small amount of concentrated hydrochloric acid, so that the use of a large amount of concentrated hydrochloric acid in the traditional process is avoided, and the problem of waste acid generated in the chloromethylation reaction process is solved; and meanwhile, the content of piperonyl butoxide in the product can be increased, and the content of piperonyl butoxide is ensured to be greater than 98%.

The invention belongs to the technical field of chemical pharmacy, and particularly relates to a preparation method and application of an impurity of a beta2 adrenal receptor stimulant and M receptor antagonist bifunctional active compound. According to the impurity preparation method of the beta2 adrenal receptor stimulant and M receptor antagonist bifunctional active compound, acetylation of amino is successfully realized by using acetylation reagents such as acetyl chloride and alkali accelerators such as N, N-diisopropylethylamine, then debenzylation is performed through hydrogenation reaction, and the compound shown in the formula I is successfully prepared. Then, through liquid chromatography purification, a high-purity compound as shown in the formula I is obtained, and the raw material medicine as shown in JKN2304 can meet the requirements of reference substances in the research and development process; the technical problem that in the prior art, an impurity synthesis process of a beta 2 adrenal gland receptor agonist and M receptor antagonist bifunctional active compound is lacked is solved.

Belongs to the technical field of pine wood nematode disease prevention and control, and particularly relates to a preparation method and application of a pyrazole-chitosan oligosaccharide derivative. Chloroacetyl chloride serves as an acylating agent, chitosan oligosaccharide is acetylated, and chloroacetyl chitosan oligosaccharide is generated; then, a pyrazole molecule with nematicidal activity is connected to the Cl site of the chloracetyl chitosan oligosaccharide through ammonolysis reaction, and the novel pyrazole-chitosan oligosaccharide derivative is obtained. The derivative has relatively high contact activity on pine wood nematodes, and LC50 of 24 hours and LC50 of 48 hours are 4.814 mM and 4.061 mM respectively; the chitosan oligosaccharide can remarkably inhibit multiple physiological indexes such as movement, feeding and service life of the pine wood nematodes, and is good in stability, low in molecular weight of the chitosan oligosaccharide, good in water solubility, green and environment-friendly, and the plant toxicity is remarkably reduced. The derivative has a good application prospect in the aspect of controlling the pine wood nematode disease and can be applied to prevention and control of the pine wood nematode disease.

The invention discloses a preparation method of antibacterial modified polylactic acid for a packaging material, and belongs to the technical field of functional modification of polylactic acid.The preparation method comprises the steps that an antibacterial barrier type polylactic acid composite material is prepared through ring opening polymerization of an initiator, grafting of antibacterial molecules and blending of montmorillonite, a chlorine-terminated initiator is generated from ethanolamine and chloroacetyl chloride, and the antibacterial modified polylactic acid is prepared; the preparation method comprises the following steps: initiating ring-opening polymerization of L-lactide to form polylactic acid with terminal group activity, covalently grafting terminal group chlorine with an antibacterial modifier through nucleophilic substitution, endowing the polylactic acid with antibacterial property, coupling modified montmorillonite with silane through organic intercalation, and then carrying out melt blending with the modified polylactic acid with antibacterial property to form a layered barrier structure and enhance interface bonding. Therefore, the film has the advantages of high barrier property, high tensile strength, excellent antibacterial activity and good degradability.

The utility model provides an acetoxyacetyl chloride synthesizer which comprises a first synthesis kettle and a second synthesis kettle, the top of the first synthesis kettle and the top of the second synthesis kettle are both communicated with a first metering tank and a second metering tank through pipelines, and the first metering tank and the second metering tank are both provided with feeding pumps. The bottom of the first synthesis kettle and the bottom of the second synthesis kettle are communicated with a rectifying kettle through pipelines, a rectifying assembly is arranged at the top of the rectifying kettle, and a discharge port is formed in the bottom of the rectifying kettle; the whole device is simple in structure, the two synthesis kettles can be alternately used, so that the production efficiency is effectively improved, acidic mixed waste gases such as sulfur dioxide and hydrogen chloride are not generated, the utilization rate of raw materials theoretically reaches 100%, the device completely conforms to an environment-friendly and pollution-free green process, the reaction process is mild, and the production cost is low. The reaction speed can be controlled by controlling the temperature and the catalyst input amount, the production operation is safe, the production cost is low, and the benefit is high.

The invention discloses a method and system for continuously synthesizing 2, 4-dichloroacetophenone, and the method for continuously synthesizing 2, 4-dichloroacetophenone comprises the following steps: S1, mixing m-dichlorobenzene and a catalyst to form a turbid liquid, and continuously inputting the turbid liquid into a tubular reactor; s2, enabling gas-phase acetyl chloride to pass through a micro-interface generator to form micron-sized microbubbles, continuously inputting the micron-sized microbubbles into a tubular reactor, and carrying out mixed reaction on the micron-sized microbubbles and the turbid liquid to obtain a mixed reaction liquid; and S3, continuously inputting the mixed reaction liquid and water into a hydrolysis reactor, and carrying out hydrolysis and separation to obtain 2, 4-dichloroacetophenone. According to the invention, the traditional kettle type stirring reaction is changed into micro-interface reaction, and the mass transfer area and the total mass transfer rate among multiple phases can be multiplied, so that the reaction rate is greatly improved, the side reaction is effectively controlled, and meanwhile, the product yield, the reaction safety and the like are improved.

The invention discloses a method for preparing methyltriacetoxysilane from acetic anhydride-containing acetyl chloride distillation tailings, and relates to the technical field of organic silicon synthesis, the method comprises the following steps: adding methyl trichlorosilane and acetic anhydride-containing acetyl chloride distillation tailings into a reaction kettle, stirring and heating; after a total reflux condition is reached, maintaining total reflux for a period of time, and then starting to collect acetyl chloride; continuously heating until the collection of acetyl chloride is completed, stopping heating, and when the temperature of the kettle is reduced to room temperature, heating again and starting vacuum negative pressure; when the kettle temperature reaches a set value, stopping heating, stopping stirring, and closing vacuum negative pressure; and after the kettle temperature is reduced to room temperature, adding pretreated activated carbon, carrying out decoloration reaction, and carrying out suction filtration after the reaction is completed, thereby obtaining the product. According to the method, a large amount of acetic anhydride in the acetyl chloride distillation tailings is used as a raw material and directly reacts with methyl trichlorosilane to prepare methyltriacetoxysilane, and the quality of the obtained product is remarkably higher than that of a product prepared by a normal process.

The application discloses a method for preparing 3-methoxy-3-methyl-1-butyl acetate, and belongs to the technical field of organic compound synthesis. The method comprises the following steps: taking 3-methoxy-3-methyl-1-butanol as raw material, and respectively adopting acetic acid, acetic anhydride and acetyl chloride as acetylation reagents, and adding a catalyst or an acid-binding agent to perform acetylation reaction, so as to obtain 3-methoxy-3-methyl-1-butyl acetate. The application provides a synthesis method for 3-methoxy-3-methyl-1-butyl acetate, takes 3-methoxy-3-methyl-1-butanol as raw material, respectively adopts acetic acid, acetic anhydride and acetyl chloride as acetylation reagents, adds a catalyst or an acid-binding agent to perform acetylation reaction, and obtains 3-methoxy-3-methyl-1-butyl acetate. In view of the defect that there is no acetylation synthesis process suitable for the target product in the prior art, the related technical blank is filled.

The invention discloses a preparation process of 2-chloro-4-(methylsulfonyl)-3-methyl benzoic acid, and relates to the technical field of preparation of inorganic compounds. The invention relates to a preparation process of 2-chloro-4-(methylsulfonyl)-3-methyl benzoic acid, which comprises the following steps: reacting 3-chloro-2-methylaniline with hydrochloric acid and sodium methyl mercaptide to form an intermediate C1, reacting with acetyl chloride, catalyzing with anhydrous aluminum trichloride to form an intermediate C2, reacting with hydrogen peroxide and sodium hypochlorite to form an intermediate C4, and reacting with sodium chloride to form the 2-chloro-4-(methylsulfonyl)-3-methyl benzoic acid. The 2-chloro-4-(methylsulfonyl)-3-methyl benzoic acid is obtained after the reaction is completed.

The invention relates to the technical field of refining of high-purity boric acid, and particularly discloses a method for removing divalent metal ions in high-purity boric acid, which comprises the following steps: dissolving the high-purity boric acid in water, filtering, adsorbing by adsorbent resin, filtering to obtain a refined boric acid solution, cooling, crystallizing, evaporating, crystallizing, carrying out suction filtration, and crushing to obtain the refined boric acid. The preparation method of the adsorption resin comprises the following steps: (1) blending polystyrene master batches with acetyl chloride, dispersing, and adding Lewis acid for reaction to obtain acetylated polystyrene particles; and (2) dispersing acetylated polystyrene particles, mixing with p-aminobenzene arsenic acid to react, filtering, and washing with alcohol to obtain the adsorption resin. After the high-purity boric acid is treated by the adsorbent resin prepared by the invention, the purity of the high-purity boric acid can reach 99.99%, and the effect of removing divalent metal ions in the high-purity boric acid can be realized.

This invention relates to the field of dichloroacetic acid preparation technology, specifically a method for preparing high-purity dichloroacetic acid. The method uses anhydrous dichloroacetic acid alkyl ester or anhydrous dichloroacetyl chloride as a single raw material. The method includes: adding deionized water to a corrosion-resistant reactor, starting stirring and cooling to 10-30°C, adding the single raw material and an acidic catalyst, reacting at 40-80°C for 1-8 hours, and then refining through multi-stage separation to obtain high-purity dichloroacetic acid. The anhydrous dichloroacetic acid alkyl ester is selected from methyl dichloroacetate, ethyl dichloroacetate, propyl dichloroacetate, or isopropyl dichloroacetate. The acidic catalyst is a ZrO₂-TiO₂ supported acid solid catalyst or a complex liquid organic acid catalyst.

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 relates to the technical field of synthesis of chlorine-containing pyridine intermediates, and discloses a method for synthesizing 2, 3, 4, 5-tetrachloropyridine by using 2, 5-dichloropyridine, which comprises the following steps: step 1, preparation of 2, 5-dichloropyridine nitrogen oxide: taking 2, 5-dichloropyridine as a raw material, reacting in the presence of a catalyst and acetic acid, and then filtering to remove the catalyst to obtain 2, 5-dichloropyridine nitrogen oxide; adding an acetic acid solution of 2, 5-dichloropyridine nitrogen oxide; step 2, nitration reaction: adding sulfuric acid and nitric acid, and reacting to obtain 2, 5-dichloro-4-nitropyridine nitrogen oxide; step 3, nitrogen and oxygen removal reaction: adding acetyl chloride to replace 4-position nitro to obtain 2, 4, 5-trichloropyridine nitrogen oxide, and then adding phosphorus trichloride to remove nitrogen and oxygen to obtain 2, 4, 5-trichloropyridine; and 4, chlorination and refining: adding Lewis acid into the 2, 4, 5-trichloropyridine, reacting to obtain a 2, 3, 4, 5-tetrachloropyridine crude product, and refining the crude product to obtain the finished product 2, 3, 4, 5-tetrachloropyridine. The invention solves the problems of more byproducts and unsatisfactory product purity and yield in the prior art.

The invention discloses a high-boiling-point styryl liquid cross-linking agent, a preparation method thereof and organic medium slurry of a high-frequency and high-speed copper-clad plate. The preparation method of the high-boiling-point styryl liquid cross-linking agent comprises the following steps: carrying out Friedel-Crafts reaction on toluene and dichloroethane to obtain 1, 2-bis (methyl benzene) ethane; the preparation method comprises the following steps: carrying out Friedel-Crafts reaction on dimethyl phenylethane and acetyl chloride to obtain 1, 2-bis (methyl acetyl benzene) ethane; the preparation method comprises the following steps: carrying out reduction reaction on 1, 2-bis (methyl acetyl benzene) ethane and sodium borohydride to obtain 1, 2-bis (methyl alpha hydroxyethyl benzene) ethane; and carrying out dehydration to obtain the 1, 2-bis (methyl vinyl benzene) ethane cross-linking agent. The 1, 2-bis (methyl vinyl benzene) ethane is in a liquid state at normal temperature, has high solubility for SEBS and other film-forming resins, can reduce the solvent amount for copper-clad plate manufacturing, is a high-boiling-point cross-linking agent, and has wide application prospects.

A beta-acetylnaphthalene production device belongs to the technical field of chemical equipment and comprises a dissolving kettle, a tubular reactor, a hydrolysis liquid separation kettle and an external evaporation crystallization kettle, a dissolving kettle solid feed inlet and a dissolving kettle liquid inlet are formed in the top of the dissolving kettle, a dissolving kettle liquid outlet is formed in the bottom of the dissolving kettle, and a first constant-temperature heat exchanger is arranged on the outer wall of the dissolving kettle; a solid feeding port of the dissolving kettle is connected with a solid feeding machine through a pipeline and connected with a valve in series, a liquid inlet of the dissolving kettle is connected with a solvent storage tank through a pipeline and connected with a valve, an electronic flowmeter and a transmission pump in series, and a liquid outlet of the dissolving kettle is connected with a tubular reactor and an acetyl chloride storage tank through a first tee joint. According to the utility model, beta-acetylnaphthalene can be continuously produced in a continuous feeding and intermittent discharging manner, so that the production efficiency is improved, and the production cost is reduced; meanwhile, through the design, multiple treatment procedures are simplified in one device for treatment, the device utilization rate is increased while the device is simplified, the occupied space of production equipment is saved, and industrial popularization is facilitated.

This invention provides a method for preparing and purifying methyl isoglycyrrhizate. The preparation method includes reacting isoglycyrrhizic acid (of formula I) or its salt in a mixed solvent of methanol and methyl acetate in the presence of acetyl chloride. The purification method involves adding crude methyl isoglycyrrhizate to a mixed solvent of organic solvent and water after the reaction, heating and stirring to dissolve; then adding water dropwise, cooling to allow crystallization, and filtering to obtain a solid. This invention, by adding a certain amount of methyl acetate during the reaction, can ensure the conversion rate, control the acidity of the reaction environment, reduce the degradation of methyl isoglycyrrhizate, and greatly improve the product yield and material utilization. The purification method for methyl isoglycyrrhizate provided by this invention can efficiently remove impurity A from the product, is simple to operate, uses little solvent, has a high yield, and is environmentally friendly.

The invention discloses a composite membrane material for sewage treatment and a preparation method thereof, and belongs to the technical field of sewage treatment, and the composite membrane material is prepared by loading three layers of different network polymers on the surface of a ceramic chip; the network-like polymer is prepared by performing esterification reaction on alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin and 2, 2 '-[oxybis (ethylene glycol oxygen)] diacetyl chloride respectively; the composite membrane material for sewage treatment prepared by the invention has relatively strong adsorption performance, relatively high mechanical strength and stability, and has a good application prospect in the aspects of adsorption of refractory organic wastewater and treatment of heavy metals and ammonia nitrogen.

The invention discloses a substituted quinoline compound and a preparation method and application thereof.The preparation method includes the steps that thionyl chloride and a specific intermediate react, DCM and other solvents are adopted, and pyridine, polyphosphoric acid, ethyl alcohol, acetyl chloride and other reagents are used in the reaction process. The structure of the obtained product is confirmed by a nuclear magnetic hydrogen spectrum, bactericidal activity tests are carried out on the obtained 29 target products, and the results show that the compound has a significant inhibition effect on a variety of plant pathogens at a concentration of 50 ppm, and especially shows excellent bactericidal activity in the aspects of pyricularia grisea, sclerotinia sclerotiorum and the like. In addition, the compounds have certain herbicidal activity.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of inositol fatty acid ester. The method comprises the following steps: (1) mixing acetyl chloride and fatty acid, adding an inositol solution, heating to 80-150 DEG C while stirring under a vacuum condition, and reacting for 20-30 minutes to obtain a mixed solution; and (2) adding ethanol into the mixed solution in the step (1), stirring for 2-3 minutes, standing, layering, separating an upper solution from a lower solution, heating the upper solution at 80-110 DEG C for 5-8 minutes, adding acetyl chloride and an inositol solution, heating to 80-150 DEG C while stirring under a vacuum condition, reacting for 20-30 minutes, and merging with the upper solution to obtain the inositol fatty acid ester. The yield of the prepared inositol fatty acid ester is high.

The application belongs to the technical field of pharmaceutical chemistry synthesis, and particularly relates to a synthesis method of a fluorofelarana intermediate 2-methyl-4-acetylbenzoic acid. In the application, o-chlorotoluene and acetyl chloride are reacted under the action of anhydrous aluminum chloride to generate 4-chloro-3-methylacetophenone; the 4-chloro-3-methylacetophenone and acetonitrile are catalyzed by Ni to generate 4-acetyl-2-methylbenzonitrile; and then the 4-acetyl-2-methylbenzonitrile is hydrolyzed to generate 2-methyl-4-acetylbenzoic acid. The application has the beneficial effect that acetonitrile is used as a cyanogen to replace halogen, and a highly toxic cyanide is abandoned, so that the whole process is safer and more environmentally friendly, the production of three wastes is reduced, and the synthesis cost of 2-methyl-4-acetylbenzoic acid is greatly reduced.

The invention relates to the technical field of medicine synthesis, and particularly discloses a preparation method of a cefdil intermediate. According to the invention, trichloroisocyanuric acid (TCCA) is taken as a green chlorination reagent, and reaction solvent and temperature are selected, so that the problem that benzene ring polychlorination side reaction and aldehyde functional group nucleophilic substitution side reaction are effectively inhibited while ortho-position high-selectivity mono-chlorination of phenolic hydroxyl is realized is successfully solved; and thus, the 2-chloro-3-hydroxy-4-methoxybenzaldehyde can be obtained at a high yield. On the basis, according to the scheme, subsequent anhydridation and amidation steps are further optimized, trimethylacetyl chloride is adopted to replace a traditional highly toxic activating reagent, safety and atom economy are improved, and meanwhile continuity and high efficiency of the reaction are ensured. The whole process route is reasonable in design, simple and convenient to operate and high in safety, raw materials and reagents are easy to obtain, the total yield of the reaction and the purity of the product are remarkably improved, and the method shows a wide application prospect in large-scale industrial production of the ceftidil.

The invention discloses a biological microcapsule for repairing heavy metal pollution as well as a preparation method and application of the biological microcapsule. The biological microcapsule consists of a core material and a wall material, the core material is prepared from bacillus subtilis, aspergillus niger, azospirillum brasilense and starch; the wall material comprises modified polyethylene glycol and sodium alginate; the modified polyethylene glycol is prepared by reacting polyethylene glycol, 2-[(tert-butyl) amino] acetyl chloride hydrochloride and 2-chloroethyl sodium sulfonate. The biological microcapsule for repairing heavy metal pollution can further enrich soil heavy metal through high adsorption capacity and adsorption capacity of the wall material, remarkably reduces the degree of heavy metal pollution of soil through excellent reduction and adsorption capacity of the complex microbial inoculant, and can be widely applied to the field of heavy metal repairing of soil.

The utility model discloses a hydrogen chloride removal system suitable for a process of producing chloroacetic acid by an acetic acid method, and belongs to the technical field of glycine production. The hydrogen chloride removal system comprises a separation kettle, a condenser, a packing absorption tower and an acetyl chloride recovery tank, the separation kettle is connected with the chlorination reaction kettle, and the separation kettle is connected with the condenser; the condenser is connected with the separation kettle through a return pipe, a non-condensable gas outlet on the condenser is connected with the packing absorption tower through a non-condensable gas outlet pipe, and a vacuum pump is arranged on the non-condensable gas outlet pipe; the packing absorption tower is connected with an acetic acid inlet pipe, an upper gas phase outlet of the packing absorption tower is connected with a tail gas treatment system, and the packing absorption tower is connected with an acetyl chloride recovery tank through an acetyl chloride outlet pipe; the acetyl chloride recovery tank is connected with the chlorination reaction kettle through a recycling pipe and is also connected with the packing absorption tower through a circulating pipe. Acetyl chloride in a chloroacetic acid finished product is recovered and used for a chlorination process, so that the consumption of raw material acetic anhydride is reduced; and meanwhile, the loss amount of raw material liquid ammonia in the subsequent ammoniation process is reduced.

The application belongs to the technical field of organic synthesis, and particularly relates to a preparation method of 4,4,4-trifluoroacetyl ethyl acetate. The preparation method of the 4,4,4-trifluoroacetyl ethyl acetate comprises the following steps: first, dissolving a base in an organic solvent, adding trifluoroacetyl chloride under the condition that the temperature is not higher than 0 DEG C, reacting for 0.5-3 h, then adding ethyl acetate, heating to 20-30 DEG C, reacting for 2-6 h, then washing the reaction product with water, drying the organic phase with anhydrous sodium sulfate, and finally evaporating the organic solvent to obtain the 4,4,4-trifluoroacetyl ethyl acetate. The preparation method of the 4,4,4-trifluoroacetyl ethyl acetate is mild in condition, simple in operation, fast in reaction speed, and easy in product separation, and is suitable for industrial production.

The application discloses a battery pack fireproof and heat-insulating coating and a preparation method thereof, and relates to the technical field of fireproof coatings. The battery pack fireproof and heat-insulating coating prepared by the application comprises a composite flame-retardant charring agent, modified phenolic resin, fillers, a silane coupling agent and a defoaming agent. The modified phenolic resin is prepared by the reaction of double-end hydroxyl polyphenyl ether, amino-phenolic resin and polythioacetal. The double-end hydroxyl polyphenyl ether is prepared by the reaction of 2,6-dimethylphenol and tetramethyl bisphenol A. The polythioacetal is prepared by the polymerization of 1,3-dimercapto-2-propanol and cinnamaldehyde. The thermal stability is improved, and the coating has the ability of self-repairing. The composite flame-retardant charring agent is prepared by the reaction of a sulfonamide piperazine compound, 4,4'-dimercaptodiphenyl sulfide and diamino diphenyl methane modified ammonium polyphosphate. The sulfonamide piperazine compound is prepared by the reaction of chlorosulfonyl isocyanate and piperazine, and then the reaction with chloroacetyl chloride. The carbonization property and thermal stability of the coating are improved.

The application discloses a preparation method of 2-cyano-3-hydroxy-2-buten-(4-trifluoromethyl-phenyl)amide, which comprises the following steps: reacting a compound of formula (II) with acetyl chloride or acetic anhydride under the action of a base; wherein the base comprises sodium ethoxide and / or sodium methoxide. In the application, sodium hydride with a relatively high risk coefficient is replaced by sodium alcoholate, the operation difficulty is reduced, the yield is improved compared with sodium hydride, and the application is more suitable for industrial production.

The application discloses a method for synthesizing benoxacor, and belongs to the technical field of chemical organic synthesis. The method comprises the following steps: taking DMF as a solvent, fully reacting ortho-nitrophenol with monochloroacetone and alkali at a certain temperature, centrifuging after the reaction is completed, obtaining a first filter cake and a DMF solution of 2-nitro-2-phenoxypropanone, removing part of the DMF through vacuum distillation, detecting the content of chloroacetone in the gas chromatograph, and adjusting the mass concentration of the 2-nitro-2-phenoxypropanone DMF solution to 10-20% after the content of chloroacetone is detected to be lower than 0.02% by using the area normalization method; then, adding Raney nickel into the 2-nitro-2-phenoxypropanone DMF solution, and performing hydrogenation reaction by passing hydrogen; after the reaction is completed, the upper clear liquid is extracted, and 3,4-dihydro-3-methyl-2H-1,4-benzoxazine DMF solution is obtained through filtration; then, an acid-binding agent alkali is added, and acylation reaction is performed by dropwise adding dichloroacetyl chloride, so as to synthesize benoxacor. The method can greatly simplify the operation process of frequently changing solvents in the process of synthesizing benoxacor, and can avoid the generation of a large amount of waste brine.

The invention discloses a synthesis method of high-quality phenylacetyl chloride, and belongs to the technical field of synthesis of phenylacetyl chloride. According to the method, the crude phenylacetyl chloride is purified by combining the strong-polarity aprotic solvent dimethyl sulfoxide and the disubstituted ionic liquid, the solvent is strong in polarity, can remove high-polarity colored group impurities, does not contain reactive hydrogen and does not react with phenylacetyl chloride, and the phenylacetyl chloride and the solvent are separated by standing and layering after mixing at normal temperature. A double bond and a benzene ring in the disubstituted ionic liquid can form a pi-pi accumulation effect with macromolecular impurities containing conjugated systems such as oligomers in the impurities, ester groups can form stable hydrogen bonds with strong hydrogen bond donors such as aldehyde groups in the impurities, ether bonds can adsorb thioether impurities, and the adsorption capacity is further enhanced through SbF6 anions. The purity of the phenylacetyl chloride synthesized through the method reaches 99.0% or above through liquid phase analysis, and the phenylacetyl chloride does not change color through high-temperature tests and completely meets the standard of high-quality phenylacetyl chloride.

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.

This application relates to the field of high-purity boric acid refining technology, specifically disclosing a method for removing divalent metal ions from high-purity boric acid, comprising the following steps: high-purity boric acid is dissolved in water and filtered, adsorbed by an adsorption resin, filtered again to obtain a refined boric acid solution, and then subjected to cooling crystallization and evaporation crystallization, filtered, and pulverized to obtain refined boric acid. The preparation steps of the adsorption resin include the following: (I) polystyrene masterbatch is mixed with acetyl chloride, dispersed, and reacted with Lewis acid to obtain acetylated polystyrene particles; (II) the acetylated polystyrene particles are dispersed, mixed and reacted with p-aminophenylarsonic acid, filtered, and washed with alcohol to obtain the adsorption resin. After treatment with the adsorption resin prepared in this application, the purity of high-purity boric acid can reach 99.99%, and the effect of removing divalent metal ions from high-purity boric acid can be achieved.