260 results about "Bromobenzenes" patented technology

The invention discloses a crown ether functionalized covalent organic framework material as well as a preparation method and application thereof, and the method comprises the following steps: adding a covalent organic framework material, 4-bromobenzo-15-crown-5, potassium carbonate and potassium iodide into an acetone solution for reaction, washing the obtained crude product, performing Soxhlet extraction with tetrahydrofuran for a certain time, and drying to obtain the crown ether functionalized covalent organic framework material. The crown ether functionalized covalent organic framework material is obtained. Compared with a synthesis method of crown ether functionalized COFs in the prior art, the method has the advantages that the crown ether (4-bromobenzo-15-crown-5) can be grafted to the COFs in one step, the Na < + > adsorption capacity and the adsorbent recycling performance are greatly improved, the synthesis method is simple, and synthesis of the crown ether functionalized COFs is greener, more convenient and more economical.

The invention discloses a preparation method of alplsutentan and an alplsutentan intermediate, alplsutentan is obtained by taking a compound SM1 as a raw material through a one-step method or a multi-step method, and the multi-step method comprises the following steps: reacting the compound SM1 with a compound SM2 to obtain an intermediate I; reacting the intermediate I with 2-[(5-bromo-2-pyrimidinyl) oxy] ethanol to obtain an intermediate II, or reacting the intermediate I with ethylene glycol to obtain an intermediate I-b, and then reacting with 5-bromo-2-chloropyrimidine or 5-fluoro-2-chloropyrimidine to obtain the intermediate II; and finally, removing a protecting group from the intermediate II to obtain alpoxivan. The one-step method comprises the following steps: when X in a compound SM1 is a fluorine atom, the compound SM1 is 5-(4-bromophenyl)-4, 6-difluoropyrimidine, and the compound SM1 reacts with sulfonamide and 2-[(5-bromo-2-pyrimidinyl) oxy] ethanol to directly obtain alpoxivan. The synthesis route is short, and the reaction conditions are mild.

The invention discloses a synthesis process of chiral cyclic ether indole. The synthesis process comprises the following steps: reacting 4-bromobenzaldehyde with malonic acid under the catalysis of piperidine to generate olefin carboxylic acid CHP-1; carrying out condensation reaction to prepare CHP-2; under the catalysis of a copper reagent, carrying out Michael addition reaction to obtain CHP-3; preparing a chiral alcohol intermediate CHP-4 through a reduction reaction; trifluoromethanesulfonic acid is used, and a chiral ether intermediate CHP-5 is prepared through ring closing; reacting with protected hydrazine by using a copper ion catalyst to obtain an intermediate CHP-6; the method comprises the following steps: by taking alcohol as a solvent, adding strong acid, and removing a protecting group of hydrazine to obtain an intermediate CHP-7; and carrying out ring closing by taking lewis acid as a catalyst to obtain an indole product CHP-8. The use of a noble metal catalyst palladium is avoided, and the cost is greatly reduced. The chiral center is directly constructed through a chemical method, and SFC is not needed for resolution, so that the cost is remarkably reduced, and industrial production is successfully realized.

The invention relates to the technical field of chemistry, in particular to a synthesis process of 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride, which comprises the following steps: by taking 4-fluoro-3, 5-dimethylbromobenzene as a raw material and hydrazine hydrate as a hydrazine source, matching with alkali such as potassium hydroxide, sodium hydroxide or potassium phosphate and the like, reacting at the temperature of 60-80 DEG C to obtain the 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride. The preparation method comprises the following steps: by taking copper or nickel source catalysts such as cuprous bromide, cuprous iodide, nickel salicylate and the like, N, N-bis (2, 6-dimethylphenyl) oxamide as a ligand, hexadecyl trimethyl ammonium bromide as a stabilizer and a dioxane-water mixed system as a solvent, reacting at 80-110 DEG C under the protection of nitrogen, separating a reaction mixed solution after the reaction is finished, and separating the reaction liquid to obtain the target product. And purifying to obtain a finished product of the 4-fluoro-3, 5-dimethyl phenylhydrazine hydrochloride. Therefore, the problems that the synthesis of the 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride is poor in safety, low in production efficiency, poor in environmental friendliness, small in substrate application range and the like are solved.

The invention discloses a method for synthesizing a platinum-based nitrogen-doped graphdiyne catalyst based on an atomic layer deposition technology and application of the platinum-based nitrogen-doped graphdiyne catalyst. Firstly, hexabromobenzene and calcium carbide are subjected to vacuum ball milling, calcination and purification to obtain a graphdiyne carrier, then the graphdiyne carrier and melamine are mixed and calcined to achieve nitrogen doping of the carrier, and then loading of platinum nanoparticles is accurately controlled through an atomic layer deposition technology. According to the method, the characteristics of an atomic layer deposition technology are utilized, deposition parameters and the number of cycles are controlled, uniform distribution and size control of Pt nano-particles on porous graphdiyne are achieved, and a nitrogen-doped graphdiyne carrier and the platinum nano-particles have a synergistic effect. The platinum-based nitrogen-doped graphdiyne catalyst prepared by the invention has the specific surface area of 734.8 m < 2 > g < 1 > and the average pore size of 8.68 nm, and shows excellent electrocatalytic activity and dynamic performance in reaction.

The present invention discloses a covalent organic polymer fluorescent probe, and the preparation method is as follows: 2,7-dibromopyrene and 1,2,3,4,5,6-hexa(4-bromophenyl)benzene are added to an organic solvent to dissolve, a Ni(0) catalyst is added, and the reaction is heated overnight. After the reaction is completed, it is cooled to room temperature, an HCl aqueous solution is added, the resulting precipitate is filtered, and washed with an organic solvent to finally obtain the covalent organic polymer fluorescent probe. The fluorescent probe is synthesized by a nickel-catalyzed Yamamoto reaction, has a significant quenching effect on nitro explosives containing OH groups, can be observed with the naked eye to have a significant color change, has high sensitivity, and has a low detection limit; and has no significant response to nitro explosives containing OH groups. Therefore, this fluorescent probe can be used as a specific fluorescent probe for highly selective detection of nitro explosives containing OH groups.

The present invention provides a paroxysmal hemoglobinuria indication drug ipropam key intermediate synthesis method, and relates to the technical field of ipropam, the method comprises: taking p-bromobenzaldehyde as an initial raw material, adopting an S-configuration catalyst to obtain an intermediate 03, carrying out protection group removal on the intermediate 03, carrying out automatic ring closing to obtain an intermediate 04, and carrying out post-treatment to obtain the paroxysmal hemoglobinuria indication drug ipropam key intermediate. Reducing the intermediate 04 with sodium borohydride to obtain a single cis-configuration intermediate 05, then carrying out a chiral flip reaction and hydrolysis to remove p-nitrobenzoic acid, then carrying out an etherification reaction with diethyl sulfate to obtain an intermediate 08, reducing amide of the intermediate 08 with sodium borohydride and boron trifluoride diethyl etherate to obtain an intermediate 09, then carrying out an acetylation reaction to protect amino, and finally carrying out a reaction to obtain the chiral cis-configuration intermediate 03. Cuprous cyanide is subjected to a cyanation reaction and a hydrolytic esterification reaction to obtain the ipropam key intermediate TM. The method is low in raw material price, high in chiral control selectivity, easy in reaction condition control and low in equipment requirement, avoids column chromatography and other operations, and is more suitable for industrial production.

The invention provides a synthesis method of an OLED polycyclic fused thiophene compound, and relates to the technical field of material synthesis, and the synthesis method comprises the following steps: providing and mixing 2-naphthalene sulfonic acid and dichloromethane, dropwise adding an N-bromosuccinimide solution into the mixture under the protection of inert gas, and reacting to obtain an intermediate A; dissolving the intermediate A, then adding sodium hydroxide, 4-bromophenylboronic acid, water and tetrakis (triphenylphosphine) palladium, and reacting to obtain an intermediate B; dissolving the intermediate B, adding sulfonic acid and phosphorus pentoxide, and reacting to obtain an intermediate C; adding the intermediate C into tetrahydrofuran, dissolving, adding lithium aluminum hydride under inert gas, and reacting to obtain a target compound. According to the method, the chemical reaction efficiency of the intermediate C is high, and the yield and LC purity of a target product are relatively high.

The invention relates to the technical field of catalytic synthesis, in particular to a chloromethylation catalyst, a preparation method of the chloromethylation catalyst and a method for preparing high-purity ortho-position, meta-position and para-position chloromethyl styrene through the chloromethylation catalyst, and the chloromethylation catalyst is prepared by loading sulfonic acid compounds and (or) pyridine compounds and (or) copper salt on a molecular sieve. The method can improve the localization selectivity of chloromethylation. The method for preparing high-purity ortho-position, meta-position and para-position chloromethyl styrene comprises the following steps of: reacting beta-bromophenylethane, paraformaldehyde and lewis acid in the presence of the chloromethylation catalyst to generate chloromethyl beta-bromophenylethane, and then performing elimination reaction under an alkaline condition to generate a chloromethyl styrene crude product; the high-purity ortho-position, meta-position and para-position chloromethyl styrene is obtained after the crude product is rectified, the brand-new catalyst is adopted in the method, the reaction selectivity is enhanced, the process is simple, and industrial production is facilitated.

This invention discloses an analytical method for benzothiazole contaminants, comprising the following steps: detection by high performance liquid chromatography (HPLC), with the following chromatographic conditions: a phenylhexyl column as the stationary phase, mobile phase A being water, mobile phase B being acetonitrile, and gradient elution; wherein the benzothiazole contaminants are at least one of 2-aminobenzothiazole, 2-hydroxybenzothiazole, benzothiazole, 2-methylbenzothiazole, 2-mercaptobenzothiazole, 2,5-dimethylbenzothiazole, 2-cyanobenzothiazole, ethyl 2-carboxylate benzothiazole, 2-chlorobenzothiazole, 2-bromobenzothiazole, 2-methylthiobenzothiazole, phenylthiocyanate, N-tert-butyl-2-benzothiazole sulfenamide, 2-(2-hydroxyphenyl)-benzothiazole, N-cyclohexyl-2-benzothiazole sulfinamide, dibenzothiazole disulfide, and N,N-dicyclohexyl-2-benzothiazole sulfonamide.

The invention discloses a method for preparing 3-phenanthrenol. The method comprises coupling a compound 3-tert-butoxyphenylboronic acid and o-bromobenzaldehyde to obtain 3'-tert-butoxy-[1,1'-biphenyl]-2-formaldehyde, then reacting 2-(chloromethoxy)-2-methylpropane with magnesium chips in tetrahydrofuran to generate a Grignard reagent, followed by substitution with 3'-tert-butoxy-[1,1'-biphenyl]-2-formaldehyde, and reflux and water separation with p-toluenesulfonic acid to obtain 3'-tert-butoxy-2-(2"-tert-butoxyvinyl)-1,1'-biphenyl, and finally ring closure with methanesulfonic acid and de-tert-butylation to obtain 3-phenanthrenol. The method introduces tert-butyl protection, thereby increasing steric hindrance and reducing isomers during ring closure, and facilitating deprotection conditions. The obtained product can have a purity of more than 99.0% without the need for column chromatography.

The application relates to a metal organic tetrahedral cage compound, a preparation method and application thereof, and belongs to the technical field of fine chemical industry. The metal organic tetrahedral cage compound is obtained by reacting a rare earth metal cerium salt with H4BPDS as a ligand 3+ As a node, H4BPDS is used as a ligand. The metal organic tetrahedral cage compound prepared by the application has low raw material price, high yield, stable chemical properties, and can efficiently catalyze the reaction of aryl iodide and aryl sulfinate to prepare diaryl sulfone derivatives under mild light and warm conditions. For the catalysis of the reactions of 4-bromo-iodobenzene and 4-methylphenyl sulfinate sodium to prepare 4-bromophenyl-4-methylphenyl sulfone, 3-bromo-iodobenzene and 4-methylphenyl sulfinate sodium to prepare 3-bromophenyl-4-methylphenyl sulfone, and 4-bromo-3-fluoro-iodobenzene and 4-methylphenyl sulfinate sodium to prepare 4-bromo-3-fluorophenyl-4-methylphenyl sulfone, the yield can reach 95% at the highest.

The invention relates to a pinoxaden preparation method, which comprises: S1, carrying out a cyclization reaction on hydrazine hydrate and a compound represented by a formula (I) to generate an intermediate 1; s2, reacting the intermediate 1 with a compound as shown in a formula (II) in the presence of alkali to generate an intermediate 2; s3, enabling the intermediate 2 to react with 2, 6-diethyl-4-methyl bromobenzene under the action of a catalyst to generate an intermediate 3; s4, the intermediate 3 and pivaloyl chloride react in the presence of alkali, pinoxaden is obtained, the structural formula of the intermediate 1 shown in the formula (I) is shown in the description, the structural formula of the intermediate 2 shown in the formula (II) is shown in the description, and the structural formula of the intermediate 3 shown in the description is shown in the description.

The invention belongs to the field of medicinal chemistry, and relates to an indole allylamine amide derivative as well as a preparation method and application thereof. Functional activity screening of G protein dependent signaling pathways is carried out on all the synthesized compounds, and it is found that the new derivatives can be used for preparing beta2-adrenergic receptor allosteric antagonism regulator drugs. Trans-indole allylamine is used as a raw material, amide coupling is performed to obtain the novel indole allylamine amide derivative, and R1 is any one of phenyl, m-methylbenzene, m-methoxyphenyl, m-bromophenyl, m-chlorphenyl, m-fluorophenyl, o-methoxyphenyl, p-methoxyphenyl, naphthalene ring, oxazole, cyclohexyl, cyclopentyl, methyl, ethyl and isopropyl. A biological activity test result shows that the indole allylamine amide derivative disclosed by the invention has relatively good antagonistic activity on beta2AR and can be used for carrying out negative allosteric regulation on the functional activity of isoproterenol.

The application discloses a conjugated polymer material capable of realizing neutral state green / black-transparent electrochromic performance and a preparation method and application thereof. The conjugated polymer material (IV) is prepared through copolymerization of a cyclic ether modified p-dibromobenzene ring monomer (I), a thiophene derivative ProDOT monomer (II) and a D-A-D unit ProDOT-BTD-ProDOT coupling monomer (III). The electrochromic polymer thin film processed from the conjugated polymer material has application prospects in the fields of intelligent windows, intelligent glasses, displays, electronic paper and the like. In the material, the cyclic ether modified p-dibromobenzene ring monomer effectively reduces the oxidation potential of the conjugated polymer, improves the electrochromic performance of the black / green-transparent electrochromic thin film, and realizes stable and reversible conversion.

The invention discloses a preparation method of a 3-substituted isocoumarin compound, and belongs to the technical field of coumarin compound synthesizing.The preparation method comprises the steps that a 2-bromophenylboronic acid compound and alkyne serve as reaction substrates, a bidentate nitrogen ligand is added and dissolved in a solvent, under the action of alkali and a copper catalyst, a normal-pressure one-step cyclization reaction is conducted in the CO2 atmosphere, and the 3-substituted isocoumarin compound is obtained. The 3-substituted isocoumarin compound is obtained. According to the method, CO2, alkyne and 2-bromophenylboronic acid are used as reaction raw materials, cheap copper is used as a catalyst, the use amount is small, the 3-substituted isocoumarin is obtained through carbon-carbon coupling-cyclization by a CO2 activation one-step method under normal pressure, the conditions are mild, the cost is low, and the method is environmentally friendly.

The invention discloses a preparation method of a covalent organic framework photocatalyst for photocatalytic reduction of CO2, which comprises the following steps: adding 4, 4 ', 4' '-(1, 3, 5-triazine-2, 4, 6-triyl) triphenylamine and 2, 5-dibromobenzene-1, 2, 4, 5-tetracarboxylic dianhydride into a reaction kettle, then adding 1-hydroxy-3-methylbenzene and isoquinoline, and uniformly mixing; and carrying out microwave heating on the reaction kettle, cooling to room temperature, filtering, collecting precipitate, washing, and then carrying out Soxhlet extraction and vacuum drying to obtain the covalent organic framework photocatalyst. A surface halogen atom modification strategy is designed and used for regulating and controlling electron distribution and light capture capacity of a donor-acceptor (D-A) in TzPm-COF, and results show that the strategy can effectively improve photocatalytic activity and selectivity of reduction of CO2 into CO, and can be applied to preparation of the TzPm-COF catalyst. A reasonable design strategy is provided for developing a functional modified COFs material for efficiently and selectively photocatalytic CO2 reduction.

The invention discloses (E)-1, 4-diether olefin and a preparation method thereof, and the (E)-1, 4-diether olefin is obtained by using 1, 3-diene as a raw material and carrying out electrochemical reaction in the presence of an electrolyte and a solvent, wherein the 1, 2, 4-trimethyl-1, 3- The structural formula of the 1, 3-diene is as follows: R1 is phenyl, p-fluorophenyl, p-chlorphenyl, p-bromophenyl, p-methylphenyl, p-methoxyphenyl, p-trifluoromethylphenyl, p-trifluoromethoxyphenyl, p-acetoxyphenyl, p-methyl formate phenyl, p-cyanophenyl, p-pinacol borate phenyl, p-phenylphenyl, o-oxybenzyl phenyl and o-methoxyphenyl; r1 is one of 1, 2-naphthyl; the solvent is a mixed solvent containing methanol. The preparation method of (E)-1, 4-diether olefin has high E-selectivity and 1, 4-selectivity, and an electro-catalysis mode is adopted, so that the use of a stoichiometric toxic, expensive or dangerous oxidant is avoided.

The invention discloses polyurethane automobile finish paint and a preparation method thereof, and relates to the field of automobile finish paint. When the polyurethane automobile finish paint is prepared, titanium dioxide, 3-butene-1, 2-diol and 6-bromine-3-(4-bromophenyl)-2, 4-dihydro-1, 3-benzoxazine are uniformly mixed, and modified titanium dioxide is prepared; carrying out formylation on microcrystalline cellulose, and grafting n-butyric acid, acetic anhydride and 2-aminopiperazine to obtain modified cellulose; the preparation method comprises the following steps: reacting 1, 3, 5, 7-tetramethylcyclotetrasiloxane with vinyl pentamethyldisiloxane to obtain single-ended vinyl hydrogen-containing silicone oil; acrylic acid, methyl acrylate, hydroxypropyl methacrylate and single-ended vinyl hydrogen-containing silicone oil are subjected to copolymerization, and modified acrylic resin is prepared; and uniformly mixing the modified acrylic resin, the modified cellulose, the modified titanium dioxide and various assistants to prepare the polyurethane automotive finish. The polyurethane automobile finish paint prepared by the invention has excellent quick-drying property, impact resistance and aging resistance.

The application provides a preparation method of 2-aminopyridopyrimidinone compounds, which comprises the following steps: reacting 2-bromo-N-phenyl nicotinamide compounds and monocyanoamine in an organic solvent in the presence of alkali to obtain 2-aminopyridopyrimidinone compounds. The method has the advantages of no metal catalysis, mild reaction conditions, high atom economy, wide substrate applicability and simple operation, and has important application value in the fields of medicinal chemistry and organic synthesis.

The present invention discloses a method for synthesizing 2-bromo-6-hydroxybenzaldehyde, belonging to the field of fine chemical technology. 2,6-dibromobenzaldehyde is used as the raw material, first protected by the aldehyde group, then borated and oxidized with hydrogen peroxide to produce 2-bromo-6-hydroxybenzaldehyde. This method has a short process, high yield, and mild reaction conditions, avoiding the harsh reaction conditions of literature methods, has potential technical advantages, and is suitable for industrial scale-up production.

The invention discloses a synthesis method of 2-butyl-3-(4-hydroxybenzoyl) benzofuran, and relates to the technical field of amiodarone intermediates.The synthesis method comprises the following steps that 2-bromoanisole and 1-hexene-2-alcohol are dissolved in a first solvent, and a first catalyst is added for a reaction; cooling to 25 DEG C, adjusting the pH value to 9-10, adding a catalyst II for reaction, and removing impurities after the reaction is completed, so as to obtain 2-butylbenzofuran; 2-butylbenzofuran and a catalyst III are added into a solvent II, vacuumizing is performed after nitrogen replacement, carbon dioxide is introduced to 0.02-3 MPa for a reaction, impurity removal treatment is performed after the reaction is completed, and 2-butyl-3-(4-hydroxybenzoyl) benzofuran is obtained; compared with a synthetic route in the prior art, the synthetic method has the advantages that the reaction steps are shortened into two steps, the synthetic steps are simplified, the synthetic efficiency is improved, the process cost is reduced, meanwhile, the conversion efficiency is higher, the total yield reaches 70% or above, and the yield is improved by 15% or above compared with the yield in the prior art.

The invention belongs to the technical field of deuterated organic chemical synthesis, and particularly relates to a synthetic method of deuterated m-dibromobenzene-D4, which comprises the following steps: a, nitration reaction of deuterated benzene: enabling the deuterated benzene to react with mixed acid to generate deuterated nitrobenzene; b, performing bromination reaction on the deuterated nitrobenzene: reacting the deuterated nitrobenzene with liquid bromine by taking iron tribromide as a catalyst to generate deuterated m-bromo nitrobenzene; c, carrying out reduction reaction on the deuterated m-bromonitrobenzene: converting the deuterated m-bromonitrobenzene into deuterated m-bromoaniline by taking biboric acid as a reducing agent; and d, diazotization reaction of the deuterated m-bromoaniline: enabling the deuterated m-bromoaniline to react with cuprous bromide to generate the target product deuterated m-dibromobenzene. The deuterated m-dibromobenzene-D4 product with high purity and deuterated rate is prepared by the synthetic method, the process is simple, the raw materials are low in price and easy to obtain, and the application of the deuterated halogenated aromatic hydrocarbon serving as an intermediate in synthesis in the fields of organic photoelectricity and deuterated medicines is expanded.

The invention discloses an efficient synthesis method of brexpiprazole, which comprises the following steps: taking 4-bromo-benzothiophene and N-Boc-piperazine as initial raw materials, under the protection of nitrogen, carrying out reaction by using a supported catalyst to prepare 4-Boc piperazine benzothiophene, and then carrying out acidolysis to obtain 4-piperazine benzothiophene hydrochloride; the method comprises the following steps: reacting 3, 4-dihydro-7-hydroxy-2 (1H) quinolinone with 1-bromo-4-chloro-butane to generate 3, 4-dihydro-7-(4-chlorobutoxy)-2 (1H)-quinolinone, and then converting the 3, 4-dihydro-7-(4-chlorobutoxy)-2 (1H)-quinolinone into 7-(4-chlorobutoxy)-2 (1H)-quinolinone; then condensing with 4-piperazine benzothiophene hydrochloride to obtain a crude product of brexpiprazole; and finally, crystallizing and purifying for multiple times to obtain high-purity brexpiprazole. According to the preparation method disclosed by the invention, 4-bromo-benzothiophene and N-Boc-piperazine are taken as starting raw materials, and high-purity brexpiprazole is prepared by optimizing selection of a catalyst and conditions of each step and through an excellent purification process.

The application discloses a preparation method of o-bromoanisole. The o-bromoanisole is synthesized through three steps, anisole is used as raw material, p-sulfonic anisole is first synthesized, 2-bromo-4-sulfonic anisole is synthesized on the basis, and finally, the sulfonic group is removed to obtain o-bromoanisole. Since anisole is used as raw material, the problems of multiple by-products, low yield and low purity existing in the synthesis path of phenol are avoided. Meanwhile, all the raw materials of the application have low cost, the process steps are simple, and etherification is not needed. Meanwhile, since anisole is used as raw material, hydrobromic acid and hydrogen peroxide can be used in the intermediate step, the hydrobromic acid is oxidized to generate bromine, the reaction rate can be controlled, the reaction efficiency is improved, the waste of bromine is reduced, the purity of the prepared product can reach 99.4%, the yield reaches 96.26%, and the product can be applied on a large scale in industry.

The invention discloses a preparation method of 4-chloromethylstyrene, and belongs to the technical field of synthesis of organic intermediates. 4-bromobenzaldehyde is adopted as a raw material and reacts with ethylene glycol under the action of p-toluenesulfonic acid to generate an intermediate 1; reacting with magnesium metal to generate a Grignard reagent, reacting with acetaldehyde, and hydrolyzing to generate an intermediate 2; finally, under the combined action of methyl dichlorosilane and tri (pentafluorophenyl) boron, the product 4-chloromethyl styrene is generated. The raw materials can be obtained in the market, the reaction of dehydrating benzyl alcohol into olefin and directly chlorinating aldehyde group to generate benzyl chloride is completed by a one-step method under the combined action of methyl dichlorosilane and tris (pentafluorophenyl) boron, the operation is simple and convenient, the overall yield is high, and a route reference is provided for synthesizing the compounds.

The invention discloses a synthesis method of bis-ethyl hexyloxyphenol methoxyphenyl triazine, which relates to the technical field of organic chemistry, and comprises the following steps: preparing an intermediate I, putting zinc chloride into reaction, adding xylene for dispersion, dropwise adding the intermediate I, resorcinol and xylene solvent to obtain a yellow intermediate II crude product, and then adding the yellow intermediate II crude product into the reaction kettle to obtain the bis-ethyl hexyloxyphenol methoxyphenyl triazine. Adding the intermediate II, a xylene solvent, an acid-binding agent, chloro-isooctane and bromo-isooctane into a reaction kettle, carrying out reaction treatment to obtain a high-purity product, and carrying out sampling detection on the step 1, the step 2 and the step 3. According to the synthesis method of the bis-ethyl hexyloxyphenol methoxyphenyl triazine, p-bromoanisole and chloro-isooctane or bromo-isooctane are adopted as raw materials, the production cost is reduced, xylene is a single solvent, the problem that a mixed solvent is difficult to recycle is solved, anhydrous aluminum chloride or anhydrous zinc chloride is adopted as a catalyst, and a recrystallization technology is adopted, so that the yield of the bis-ethyl hexyloxyphenol methoxyphenyl triazine is increased. The purity of the product is improved, and the bis-ethyl hexyloxyphenol methoxyphenyl triazine with higher purity is prepared.

This invention discloses a method for synthesizing a tenapano hydrochloride intermediate. The synthesis method includes the following steps: (1) condensing the compound 3-bromophenylacetaldehyde and the compound N-methyl-(2,4-dichlorophenyl)methylamine under dehydration conditions to obtain an enamine intermediate; (2) subjecting the enamine intermediate to an intramolecular cyclization reaction in the presence of an acid catalyst to obtain the tenapano hydrochloride intermediate 4-(3-bromophenyl)-6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinoline. The synthetic route provided by this invention requires only two steps to construct the key framework, and has the advantages of short reaction steps, high overall yield, and no need to use highly toxic liquid bromine. This process has high atom economy, reduces the emission of waste gas, wastewater, and solid waste, and is suitable for large-scale industrial production under mild conditions.

This invention relates to the field of fine chemical catalysis technology, specifically to an improved ion-gel confined palladium-on-carbon catalyst, its preparation method, and its applications. The catalyst uses N,N-dimethylacetamide (DMAc) as a solvent and potassium acetate as a base, with the addition of a catalytic amount of antioxidant 168 [(tris(2,4-di-tert-butylphenyl) phosphite)], and the reaction is carried out under milder CO pressure (1.0-1.6 MPa) and temperature (90-110 °C). This improved catalyst, in synergy with the optimized process, unexpectedly enables the high conversion and selectivity of 4-bromobenzyl sulfone derivatives to 4-methylsulfonylbenzoic acid derivatives, while maintaining the catalyst's excellent recyclability and stability. This invention provides a highly efficient, green, and easily industrialized synthetic route for the target product.

The invention provides a bromine flame retardant containing secondary amine reaction sites for epoxy resin and a preparation method of the bromine flame retardant. The preparation method of the flame retardant comprises the following steps: dissolving tetrabromophthalic anhydride, adding primary amine containing a secondary amine group for reaction, and removing a solvent to obtain the bromine flame retardant containing the secondary amine, a carboxylic acid group and a bromine element at the same time. The flame retardant is liquid at room temperature and is convenient to use, and meanwhile, the molecular structure of the flame retardant contains secondary amine, carboxylic acid groups and bromine elements, so that the flame retardant can participate in an epoxy reaction, and meanwhile, a promoting effect and excellent product flame retardant performance are provided for an amine reaction.