49 results about "Nitro reduction" patented technology

The invention discloses a catalytic system for preparing amine compounds through nitro reduction and application of the catalytic system. The catalytic system comprises an alkaline aqueous solution, a reducing agent and a catalyst, the alkaline aqueous solution is an alkali metal hydroxide aqueous solution; the reducing agent is alkali metal hydroboron and / or alkaline earth metal hydroboron; the catalyst is copper salt lewis acid and / or other lewis acid; the other Lewis acid is selected from one or a combination of more of cobalt salt, ferric salt, zinc salt, manganese salt and palladium salt. When the catalytic system is used for reducing the aromatic nitro-compound, the using amount of a reducing agent is small, meanwhile, the using amount of an organic solvent is reduced, the reaction yield is high, the reaction is milder, and amplified production of the process is facilitated.

The invention discloses a synthesis method of 5-(1H-pyrrole-1-yl)-2-mercaptobenzimidazole, which comprises the following steps: carrying out cyclization condensation reaction on o-phenylenediamine and thiourea in an acidic environment provided by hydrochloric acid to obtain 2-mercaptobenzimidazole; the preparation method comprises the following steps: carrying out nitration reaction on 2-mercaptobenzimidazole, sulfuric acid and nitric acid to obtain 2-mercapto-5-nitrobenzimidazole; the preparation method comprises the following steps: carrying out nitro reduction reaction on 2-sulfydryl-5-nitrobenzimidazole and hydrogen under the catalysis of nickel to obtain 5-amino-2-sulfydryl benzimidazole; the preparation method comprises the following steps: carrying out an N-alkylation reaction on 5-amino-2-mercapto benzimidazole and tetrahydro-2, 5-dimethoxyfuran under the catalysis of copper chloride to generate 5-(1H-pyrrole-1-yl)-2-mercapto benzimidazole, and carrying out a reaction on the 5-amino-2-mercapto benzimidazole and tetrahydro-2, 5-dimethoxyfuran to generate the 5-(1H-pyrrole-1-yl)-2-mercapto benzimidazole. The method disclosed by the invention has the outstanding advantages of mild and easily-controlled conditions, simple and convenient post-treatment, high yield, economy, environmental protection, suitability for large-scale production and the like, conforms to the green chemical development concept, and has important application value.

The invention discloses a synthesis method of Olrabatinib, which comprises the following steps: by taking 2-methyl-5-nitro trifluorotoluene as a raw material, carrying out a Waller-Ziegler reaction, an alkylation / silanization reaction of amine, nitro reduction, a condensation reaction and a Caslow-Stevens coupling reaction, so as to obtain the Olrabatinib. By optimizing process conditions and a reaction system, the synthesis method disclosed by the invention has the remarkable advantages in the following aspects: the raw material cost is greatly reduced by adopting low solvent consumption; the product yield is improved by accurately controlling reaction parameters; a standardized post-treatment process is developed, and large-scale stable production is realized. According to the technical system, the technical bottlenecks of high energy consumption and high pollution in the traditional synthesis route are effectively solved, and an innovative solution is provided for green manufacturing of fine chemicals.

The application discloses a synthesis process of (-)-alpha-lycorane alkaloid and belongs to the technical field of organic synthesis chemistry. (2Z,4E)-7,7-diethoxy-3-hydroxyhepta-2,4-dienoic acid methyl ester and 3,4-methylenedioxy-beta-nitrostyrene are used as starting materials, and (-)-alpha-lycorane is obtained through catalytic asymmetric tandem Michael addition reaction, nitro reduction amination reaction, Boc amidation reaction, Bischler-Napieralski cyclization reaction, ketone enolization tandem esterification reaction, enol triflate reductive hydrogenolysis reaction and amide reduction reaction in sequence. (-)-Alpha-lycorane has a four-membered ring core skeleton of pyrrole-phenanthridine ring, has good in-vitro tumor inhibition activity and cell proliferation growth inhibition activity. The synthesis process can realize efficient, simple and full synthesis of (-)-alpha-lycorane.

The invention discloses a method for preparing nanoscale ammoniated aramid fibers through reduction after mixed acid nitration, and belongs to the technical field of chemistry and materials. The method comprises the following steps: by taking waste aramid fiber as a raw material, converting the aramid fiber into nitrified aramid fiber by utilizing nitroxyl positive ions in mixed acid; and reducing nitryl groups on the nitrated aramid fibers into amino groups by utilizing a relatively cheap tin tetrachloride catalyst under a mild condition, so as to successfully prepare the ammoniated aramid fibers. The method for preparing the nanoscale ammoniated aramid fiber through reduction after mixed acid nitration has the following advantages that operation is easy and convenient, cost is low, and industrial production is facilitated; (2) the reaction temperature is low, the experiment condition is mild, and the sustainability is realized; (3) the reaction is fast, and the period is short; and (4) the product is convenient to collect, and subsequent use is facilitated.

The application discloses a synthesis method of a trident connecting segment which can be used for improving hydrophilicity of an antibody drug conjugate, and relates to the field of organic synthesis. The {[5-amino-2-(3,3,4,4-tetramethyl-2-oxa-3-silapent-1-yl)phenyl]methyl}(methyl)amino)methane acid-2-methylpropan-2-yl ester can be used for connecting a hydrophobic dipeptide, a hydrophilic chain and a small molecule drug in an ADC drug, so as to prolong the action time of the ADC drug. The application takes cheap and easily obtained commercial raw material 2-bromo-5-nitrobenzaldehyde as a starting raw material, and successfully prepares the target product through seven steps of conventional transformation such as reduction amination, protection, coupling, ozonation and nitro reduction, with a total yield of about 60% and a scale of hundreds of grams. The starting raw material is cheap, the operation and treatment are simple, and the reaction condition is mild, so that the application is a brand-new process synthesis route, and has good economic benefits and market prospects.

The application provides a preparation method of bumetanide, taking p-chlorobenzoic acid as a starting material, performing chlorosulfonation, nitration, and ammonolysis to obtain a key intermediate of 3-(N-(tert-butyl) sulfamoyl)-4-chloro-5-nitrobenzoic acid, then performing phenoxylation, nitro reduction, n-butylation, and tert-butyl removal, and finally obtaining the bumetanide. Compared with the synthesis process of the prior art, the method has less side reactions, low cost, high yield, high safety, and is beneficial to industrial production.

The invention relates to a preparation method and application of an N-alkyl amide natural product Cubebamide and an analogue thereof, and belongs to the field of compound technologies and medicinal chemistry. According to the invention, commercially available 3, 4, 5-trimethoxybenzaldehyde 1 is used as a raw material, a compound 3 is obtained through a Horner-Wadsworth-Emmons (HWE) reaction, and then a compound 4 is obtained through hydrolysis. A compound 5a-5f is used as a raw material, a compound 6a-6f is synthesized through a Henry reaction, and a compound 8a-8f is obtained through double bond and nitro reduction. And carrying out condensation reaction on the two fragments 4 and 8a-8f to obtain the natural product Cubebamide and the analogue 9a-9f thereof. The compounds 9a, 9c and 9d disclosed by the invention have relatively good anti-inflammatory activity; the compounds 9b, 9e and 9f have remarkable anti-inflammatory activity. The synthesis method has the advantages of easily available raw materials, mild reaction conditions, environmental protection and simple operation.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of hydrogen-containing silane mediated benzoxazole derivatives, which comprises the following steps: (2-nitrophenyl) benzoate and analogues thereof as nitro substrates are dissolved in acid liquor with a palladium catalyst, hydrogen-containing silane is slowly injected, reaction is carried out under normal pressure, after the reaction is finished, a reaction product is subjected to post-treatment, and the hydrogen-containing silane mediated benzoxazole derivatives are obtained. Separating and purifying to obtain a target product benzoxazole derivative. The novel synthesis method of benzoxazole and derivatives thereof is adopted, high-pressure hydrogen and inert gas protection required by a traditional hydrogenation method is abandoned, nitro reduction and cyclization are completed in one step, and a safe, economical and environment-compatible synthesis scheme is provided for large-scale production of benzo-azacyclo drug intermediates.

The invention provides an omariglitazone intermediate, a preparation method thereof and a method for preparing an omariglitazone key intermediate, and relates to the technical field of organic chemistry. The omarignelone intermediate provided by the invention has a structure as shown in a formula VIII; the omariglitazone intermediate is easy to obtain and can be conveniently prepared by taking benzaldehyde as a starting raw material, a chiral chromatographic column does not need to be used for preparation of the omariglitazone intermediate, a key chiral center of the omariglitazone intermediate is constructed by catalyzing a cheap chiral amine catalyst through an asymmetric Knoevenagel-Michael addition reaction, and the preparation method is simple and convenient. According to the omariglitazone intermediate, industrial production of the omariglitazone key intermediate (the structure as shown in the formula I) is easy to realize, and the production cost is reduced. The invention provides a method for preparing an omariglone key intermediate (a structure shown in a formula I), the omariglone key intermediate can be prepared from the omariglone intermediate through a nitro reduction reaction, a Jappp-Klingemann reaction and an indole synthesis reaction, and the method is suitable for industrial production. A formula VIII and a formula I are shown in the description.

The application discloses a preparation method of 2-acetylamino-4-[(2-hydroxyethyl)sulfonyl]benzoic acid. The 2-acetylamino-4-[(2-hydroxyethyl)sulfonyl]benzoic acid is prepared from 4-fluoro-2-nitrobenzoic acid methyl ester as a starting material through aromatic nucleophilic substitution reaction, nitro reduction reaction, ester hydrolysis reaction, amino acylation reaction, thioether oxidation reaction and the like. The method has the advantages of mild reaction condition, high yield, low cost, easy availability of raw materials, and the like. The synthesis process meets the requirements of green chemistry, the synthesis route is innovative, the reaction post-treatment is simple, and the product is easy to purify.

The invention provides a method for synthesizing 4, 4 '-difluorobenzophenone from p-nitrobenzoyl chloride, and belongs to the field of organic synthesis. The method comprises the following steps: (1) reacting paranitrobenzoyl chloride with aromatic fluoride in the presence of a catalyst to obtain 4-nitro-4 '-fluorobenzophenone; (2) carrying out nitro reduction reaction on the 4-nitro-4 '-fluorobenzophenone obtained in the step (1) to obtain 4-amino-4'-fluorobenzophenone; and (3) carrying out diazotization reaction on the 4-amino-4 '-fluorobenzophenone obtained in the step (2), anhydrous hydrogen fluoride and sodium nitrite, and after the reaction is finished, heating and carrying out cracking reaction to obtain the product 4, 4'-difluorobenzophenone. In the synthesis process, the generation of isomers is avoided, the reaction selectivity is improved, the generation of 4-fluorobenzophenone impurities is reduced, the product purity is improved, and a guarantee is provided for the quality of downstream polyether-ether-ketone products.

The present invention relates to the technical field of camptothecin derivative preparation, particularly to a camptothecin derivative synthesis method, which uses 2-nitroacetophenone and isopropylamine as raw materials, and the camptothecin derivative is obtained through a Mannich reaction, a methylsulfonylation reaction, a nitro reduction reaction and a ring closing reaction. According to the synthetic method of the camptothecin derivative, the complex camptothecin derivative is split into two segments 1-(2-aminophenyl)-3-(N-isopropyl-N-methylsulfonylamino) propan-1-one and a compound V which are easy to prepare, and finally, a plurality of rings and chemical bonds are constructed simultaneously through one-step efficient ring closing reaction. The yield attenuation caused by progressive multiplication of the yield in the traditional linear synthesis is avoided, and the total yield is improved.

The invention relates to a preparation method and a preparation system of quinclorac, and belongs to the technical field of herbicide preparation, AuPd alloy nanoparticles are loaded on a lanthanum-doped CsPMo composite carrier, a'Lewis acid site + electron-rich metal active center 'synergistic system is constructed, lanthanum ions are embedded into Keggin structural gaps of CsPMo through ionic bonds or coordinate bonds, and the quinclorac is prepared. The specific surface area of the composite carrier is remarkably increased, the number of Lewis acid sites is increased, electron metal-composite carrier interaction between an AuPd alloy and the composite carrier induces electrons to be transferred from the carrier to the alloy, an electron-rich active center is formed, an oxygen activation energy barrier is reduced, oxygen ion active oxygen species are efficiently generated, and the catalytic activity of the AuPd alloy is improved. Meanwhile, hydrogen is accelerated to be dissociated into active hydrogen species, sufficient active species are provided for oxidation reaction and reduction reaction respectively, and efficient promotion of methyl oxidation, nitro reduction and subsequent ring closing reaction of 1-chloro-2-methyl-3-nitrobenzene is ensured.

The invention discloses a high-dispersion metal co-doped carbon catalyst and a preparation method and application thereof.The preparation method comprises the steps that S1, organic matter is adsorbed by layered double-metal hydroxide, and organic-carbon-containing micromolecule anchored layered double-metal hydroxide is obtained; and S2, carrying out heat treatment on the micromolecular anchoring layered double metal hydroxide containing the organic carbon at the temperature of 600-1400 DEG C. The catalyst is prepared by the method and can be used for catalyzing nitro reduction reaction of aromatic hydrocarbon. The high-dispersion metal co-doped carbon catalyst prepared by the invention has very high catalytic activity, stability and cycle performance, can realize magnetic separation, and is especially suitable for catalysis of reduction reaction of aromatic nitro compounds. The preparation method has the advantages of cheap and easily available raw materials and simple process, and is suitable for large-scale industrial production.

The invention relates to the technical field of pesticide preparation, and particularly discloses a novel preparation method of a key intermediate 1-(2, 4, 6-trichlorophenyl)-propyl-2-ketone of a bactericide pydiflumetofen. The method comprises the following steps: by taking 3, 5-dichloro-4-fluoronitrobenzene as a starting raw material, sequentially carrying out four-step unit reactions: reacting with ethyl acetoacetate under an alkaline condition to prepare 2-(2, 6-dichloro-4-nitrophenyl)-3-oxobutyric acid ethyl ester, and reacting with ethyl acetoacetate under an alkaline condition to prepare 2-(2, 6-dichloro-4-nitrophenyl)-3-oxobutyric acid ethyl ester; carrying out degreasing under an acidic condition, so as to obtain 1-(2, 6-dichloro-4-nitrophenyl)-propyl-2-ketone; reducing the nitro group to obtain 1-(4-amino-2, 6-dichlorophenyl)-propyl-2-ketone; and performing Sandmeyer reaction to obtain a target product. The preparation method is novel in synthetic route, few in side reaction and high in total yield, the content of a target product is larger than 99%, the preparation method is suitable for industrial production, and a key support is provided for industrialization of pydiflumetofen.

Polyimide containing dibenzofuran (thiophene) and triphenylamine structure and preparation method and application thereof, and application thereof, the present application relates to polyimide containing dibenzofuran (thiophene) and triphenylamine structure and preparation method and application thereof. In order to solve the problem of low solubility of aromatic polyimide in organic solvent, poor optical contrast, slow response time and poor capacitor performance, 2,8-dibromodibenzofuran (thiophene) is used as raw material, and 4-methoxy-4'-nitrodiphenylamine is reacted to obtain a new precursor containing dibenzofuran (thiophene) and triphenylamine structure. The nitro group is reduced to obtain a diamine monomer, which is polymerized with dianhydride to form a new high-performance polyimide. At the same time, the polymer has excellent electrochromic performance, including excellent cycle stability, fast switching time, high optical contrast and low voltage start. It also has excellent capacitor performance, including excellent specific capacity and cycle stability. The present application is expected to be applied in the field of electrochromic supercapacitor.

The present application relates to a preparation method of bumetanide, and belongs to the technical field of pharmaceutical chemistry. The present application takes 4-chlorobromobenzene as a starting material, and is subjected to sulfonylation, nitration, ammonolysis, substitution, cyanation, nitro reduction, alkylation, and finally acidification to obtain bumetanide. In the synthetic route of the present application, the carboxyl group does not need to be protected, but a cyano group which does not need functional group protection is introduced, and finally the cyano group is directly hydrolyzed into a carboxyl group to obtain bumetanide. The present application has few side reactions, the intermediates can be precipitated in water, greatly reducing the solvent cost, being easier to purify, the quality of the intermediates and bumetanide being easy to control, reducing the production risk, and being more beneficial to industrial mass production.

This invention provides a method for synthesizing milobalin benzylsulfonic acid, comprising the following steps: a chiral enone undergoes a condensation reaction with cyanoacetate in the presence of ammonium acetate to obtain an unsaturated cyano ester; next, the unsaturated cyano ester undergoes a condensation reaction with nitromethane to obtain a nitro ester; the nitro ester is then deesterified at high temperature to obtain a chiral nitro nitrile, which is then reduced to a chiral amino nitrile; subsequently, the chiral amino nitrile is hydrolyzed to obtain the free base of milobalin; finally, the free base of milobalin is salted with benzylsulfonic acid to obtain milobalin benzylsulfonic acid. This invention stereospecifically constructs a chiral cyclobutane quaternary carbon center to obtain a chiral nitro ester with a single stereoconfiguration, avoiding the chiral isomer waste generated by chiral isomer resolution, eliminating the need for chiral column separation or chiral resolution, significantly reducing production costs, and simultaneously avoiding the environmental pollution caused by residual heavy metal titanium in the product and solid waste heavy metal titanium.

The invention relates to the technical field of medicine synthesis, and particularly discloses a synthesis process of an estrogen regulating medicine. A is used as a starting point of a reaction route, J is prepared through naphthalenone reduction and enol etherification, electron-rich biaryl construction, nitro reduction and benzyl deprotection, secondary amine construction, chiral resolution, acetylation and LAH strong reduction in sequence, all the reaction raw materials are low in price and easy to obtain, the process is stable and mild, the yield is high, and the method has high value for adjusting rapid and mild synthesis of estrogen drugs.

The invention relates to the field of chemical synthesis, in particular to a synthesis method of 6-bromoindole-2-carboxylic acid. Comprising the following steps: preparing 4-bromo-2-aminotoluene; preparation of 6-bromoindole-2-carboxylic acid ethyl ester; and preparing the 6-bromoindole-2-carboxylic acid. According to the present invention, the reduction cyclization and hydrolysis process is improved, the diethyl malonate is adopted as the mild reducing agent, and the step-by-step temperature control technology is combined so as to significantly improve the yield and the purity; the invention discloses a three-step synthesis process of a bromo-indole carboxylic acid derivative. The method comprises the following steps: 1, in an improved mixed solvent system, carrying out a reduction reaction of reducing nitryl into amino; in the second step, a controllable reduction cyclization technology is adopted, and nitro amination is achieved; in the third step, the ester bond breaking efficiency is improved through the synergistic effect of alkaline hydrolysis and a solvent.

The invention discloses a preparation method of a dabigatran etexilate precursor, and belongs to the technical field of drug intermediate synthesis. The method comprises the following steps: S1, under the protection of nitrogen, reducing nitro of a compound IV into amino by taking tetrahydroxy diboron and 4, 4 '-dipyridyl as a concerted catalytic system, and purifying to obtain a compound III; s2, pretreating a compound III, a compound II and a condensing agent, performing low-temperature activation and microwave reaction in a DMF / DCM mixed solvent in the presence of HATU, HOAt and DIPEA, and performing post-treatment and recrystallization to obtain an amino amide intermediate; and S3, dissolving the amino amide intermediate in glacial acetic acid, carrying out reflux cyclization, and carrying out post-treatment and recrystallization to obtain a compound I. According to the invention, tetrahydroxy diboron and 4, 4 '-dipyridyl are adopted to synergistically catalyze nitro reduction, the conditions are mild, and the reaction is rapid; by means of synergistic catalysis of HATU and HOAt, water removal through a 4molecular sieve, batch addition of HATU, microwave assistance and the like, the reaction time is shortened, the yield is increased, side reactions are reduced, and the method is suitable for industrial production.

The invention relates to the technical field of orientation agents, in particular to a low-temperature orientation agent material. The low-temperature orientation agent material is prepared by the following steps: performing Suzuki coupling reaction on 4-broronitrobenzene and 4-perfluorohexyl butyl boric acid to prepare an intermediate A, performing nitro reduction to obtain an intermediate B, and finally performing ureation reaction on the intermediate B and isocyanate ethyl acrylate to obtain the low-temperature orientation agent material. The low-temperature orientation agent can be used for preparing a constant-transparent mode dimming film; the normally transparent mode dimming film is prepared by coating a composition containing a microcrystal composition, a polymerizable composition, a photoinitiator and the orientation agent between two layers of PET-ITO conductive films and carrying out ultraviolet curing and other processes, and the middle layer is a vertical orientation polymer microcrystal layer. A traditional PI layer technology is not needed, the production process is simplified, the orientation agent can still stably anchor and induce orientation at low temperature, the dimming performance and durability of the dimming film can be improved, and the application range of the dimming film in a low-temperature scene is effectively widened.

The invention discloses a production system and a production method of medicinal p-aminobenzoic acid. The production system comprises a filter column, a hydrogenation reaction kettle, a catalyst filter, a tubular hydrogenation reactor, a fine filter and a crystallization kettle, the production method comprises the following steps: pumping p-nitrobenzoic acid and a solvent into a hydrogenation reaction kettle through a filter column, and reacting until 3-5% of raw materials are left; then pressing out the material from the hydrogenation reaction kettle, enabling the material to enter a tubular hydrogenation reactor through a catalyst filter for continuous reaction until the material is completely reacted, finally filtering the liquid material through a micro-filter, and enabling the liquid material to enter a crystallization kettle for crystallization. On one hand, a small amount of residual colored impurities, heavy metal impurities and insoluble tiny foreign matters in raw materials are removed by adopting a multi-effect filter column, and on the other hand, hydrogenation reaction is carried out by adopting a manner of connecting a kettle type reactor and a tubular reactor in series; the content of intermediate-state impurities in nitro reduction and the content of impurities in side reactions such as decarboxylation and polymerization can be effectively reduced, and finally para aminobenzoic acid meeting the medicinal-grade requirement can be obtained.

The application discloses a method for photo-induced nitro reduction hydrogenation, and belongs to the field of medical compound synthesis.The method provided by the application takes iron trichloride and palladium-carbon as the catalysts of main reactions, and realizes nitro reduction into amino under the conditions of normal temperature, normal pressure and nitrogen, the reaction has high catalytic efficiency and fast reaction rate, the reaction time is only 10 minutes, the yield of the product obtained by nitro reduction is high, the experimental cost is greatly reduced, the method is suitable for the synthesis and amplification of later-stage compounds, the method has simple steps, wide substrate application range, and the effects of high efficiency, green environmental protection, safety and cost saving, and the reaction has fast reaction rate, and has excellent application prospect in industrial production.

The application discloses a preparation process of bumetanide. 4-chloro-3-nitro-5-sulfamoylbenzoic acid is used as a starting material, and nucleophilic substitution is carried out with phenol in potassium hydroxide aqueous solution to obtain a compound with a structural formula Int01; in a methanol-water mixed solvent, palladium-carbon is used as a catalyst, and ammonium formate is used as a hydrogen source for transfer hydrogenation, so that the nitro group on the compound with the structural formula Int01 is reduced to an amino group, and a compound with a structural formula Int02 is obtained; the compound with the structural formula Int02 is subjected to reductive amination with n-butyl aldehyde and sodium triacetoxyborohydride to obtain a crude bumetanide product; after the crude bumetanide product is refined in an acetic acid and cyclohexane system, decolorization is carried out in methanol-water by using activated carbon, and crystallization is carried out to obtain a pure bumetanide product; and the pure bumetanide product is mixed with mannitol, an alkaline adjusting agent and taurine to obtain a finished product.

The application belongs to the technical field of biological medicine, and particularly relates to a preparation method of N-(3-bromo-5-fluoro-4-methylphenyl)acetamide. The application takes 3,4-difluoro-5-bromonitrobenzene as an initial raw material, first carries out a coupling reaction with malonic acid diethyl ester, then carries out a decarboxylation reaction in the presence of a chlorinated salt, then carries out a nitro reduction reaction in the presence of a reducing agent and a catalyst, and finally carries out amino protection by using acetic anhydride. The preparation method provided by the application obtains the target product N-(3-bromo-5-fluoro-4-methylphenyl)acetamide through four-step reactions, has high total yield of the target product, is simple to operate, has good repeatability, has few side reactions, is simple to purify, has low production cost, and is suitable for industrialized scale production. As shown in the test results of examples, the total yield of N-(3-bromo-5-fluoro-4-methylphenyl)acetamide prepared by the preparation method provided by the application is 78.4%.

The invention relates to the technical field of photoresist, in particular to photoresist for a capacitive touch sensor and a preparation process of the photoresist. The invention discloses a preparation process of photoresist for a capacitive touch sensor. The preparation process comprises the following steps: preparing a modified photoreaction agent; preparing modified polyimide resin powder; preparing silicon dioxide hollow carbon spheres and nano titanium dioxide hybrid particles; and preparing the photoresist. The preparation method comprises the following steps: firstly carrying out nitration reaction on 4-tert-butylphenol, then reducing nitryl into amino to obtain amino substituted 4-tert-butylphenol, protecting the amino by di-tert-butyl dicarbonate ester, then oxidizing iodobenzene into a high-valence iodine active intermediate by taking m-chloroperoxybenzoic acid as an oxidizing agent, and reacting with Boc-amino substituted 4-tert-butylphenol to obtain the high-valence iodine-substituted 4-tert-butylphenol. And finally, carrying out a replacement reaction with silver trifluoromethanesulfonate, carrying out deprotection to obtain a modified photoreaction agent, and carrying out a condensation polymerization reaction on the modified photoreaction agent, 4, 4 '-hexafluoroisopropyl phthalic anhydride and the like to generate a polyamic acid prepolymer, so that the photoetching resolution can be greatly improved.

The invention discloses a green preparation method of 3, 5-dichloroaniline based on a pipeline reaction. The method comprises the following steps: dissolving 3, 5-dichloronitrobenzene in a water-alcohol mixed solvent, and adding a stabilizer; feeding the obtained solution into a continuous pipeline reactor, introducing hydrogen into a first-section catalytic zone, and selectively reducing nitro groups by using a Pd / C-Fe2O3 catalyst; ammonia gas is introduced into the second-section catalytic zone, and directional ammoniation is carried out by using a Ni-B catalyst; a neutralizing solution and a sodium lactate trapping agent can be injected between the two sections to stabilize the intermediate; and carrying out flash evaporation and membrane separation treatment on the reaction product, and recycling the solvent, the stabilizer and unreacted gas to obtain the 3, 5-dichloroaniline with the purity of more than or equal to 99%. According to the method, efficient coupling of nitro reduction and ammonification reaction is realized through division and cooperation of Pd / C-Fe2O3 and Ni-B dual catalysts and combination of partitioned temperature control and intermediate stabilization measures, the proportion of by-products is remarkably reduced, the yield and the purity are improved, and the service life of the catalysts is prolonged.