39 results about "Iodobenzene" patented technology

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 discloses a COF-based heterogeneous iodobenzene catalyst and its preparation method and application, belonging to the field of catalyst preparation technology. The COF-based heterogeneous iodobenzene catalyst is obtained by polymerizing a hydrazide monomer containing an iodophenyl group unit and 1,3,5-tris(4-formylphenyl)triazine; the structural formula of the hydrazide monomer containing an iodophenyl group unit is: The COF-based heterogeneous iodobenzene catalyst can be used as a catalyst for the chlorination reaction of anisole, catalyzing the chlorination reaction of anisole, achieving heterogeneous catalysis, and using a small amount, easy to recover, improving the utilization rate of the catalyst, and reducing the cost of anisole chlorination.

The invention belongs to the technical field of angiographic contrast agents, and particularly relates to an angiographic contrast agent for corpses and a preparation method of the angiographic contrast agent. The angiographic contrast agent for the corpse is prepared from the following components in parts by mass: 20 to 35 parts of iodine-containing polymer, 30 to 50 parts of iodo-benzene ring compound, 90 to 150 parts of glycerol triacetate, 30 to 40 parts of dimer acid and 600 to 800 parts of liquid paraffin, the iodine-containing polymer is obtained by copolymerizing (methyl) C4-6 alkyl acrylate, polyethylene glycol diacrylate and an iodine-containing monomer, and the iodine-containing monomer is selected from at least one of 3-iodine-ethyl acrylate, 3-iodine-methyl acrylate and (methyl) iodobenzyl acrylate. The blood vessel contrast agent disclosed by the invention can realize an excellent blood vessel contrast effect on a corpse, can also obtain a relatively ideal contrast effect for a corpse with relatively long death time, and provides powerful support for the corpse work.

The invention provides an aryl alkyl ketoxime derivative as well as a preparation method and application thereof, and relates to the field of aryl oxime derivatives. The preparation method of the aryl alkyl ketoxime derivative comprises the following steps: by taking potassium formate as an additive, carrying out free radical reaction on a compound I and a compound II under ultraviolet irradiation in the presence of tert-butyl nitrite to obtain the aryl alkyl ketoxime derivative, the compound I is substituted iodobenzene or iodopyridine; the compound II is substituted styrene or thienyl ethylene; wherein a hydrogen atom transfer / single electron transfer relay sequence is utilized to activate a compound I, and tert-butyl nitrite is adopted as a bifunctional reagent, and is used as a hydrogen atom transfer reagent and an oxime source. According to the preparation method of the aryl alkyl ketoxime derivative, pre-functionalization is not needed, a reaction substrate is wide in universality and good in compatibility, reaction conditions are mild, operation is easy and convenient, a target product can be efficiently and rapidly prepared on the premise of high yield, and a new way is provided for oxime synthesis.

The invention provides a preparation method of iodobenzene diacetate, and belongs to the technical field of preparation of drug intermediates. According to the method, 50wt% hydrogen peroxide reacts with acetic anhydride to obtain a peracetic acid system, separation and purification are not needed, the peracetic acid system directly reacts with iodobenzene, and iodobenzene diacetate is prepared. The method has the advantages of simple and easy process, mild conditions, low production cost and less wastewater discharge, and is suitable for industrial production.

The invention belongs to the technical field of organic synthesis, and provides a synthesis method of diiodosilane. The synthesis method is carried out in a first reactor and a second reactor which are connected in series, and comprises the following steps: adding a first metal chloride, a solvent, dichlorosilane (DCS) and iodobenzene into the first reactor, and carrying out a pre-reaction; after the pre-reaction, continuously introducing a solvent, dichlorosilane and iodobenzene into the first reactor; meanwhile, enabling the pre-reaction feed liquid in the first reactor to continuously flow into a second reactor filled with a second metal chloride; the first reactor and the second reactor simultaneously react; and when the volume of the reaction material liquid in the second reactor reaches a target liquid level, continuously extracting and collecting the reaction material liquid in the second reactor to realize continuous preparation of diiodosilane. The synthesis method provided by the invention is high in dichlorosilane conversion rate.

The invention relates to the field of drug synthesis, in particular to an amine compound for fungi drugs and a preparation method of the amine compound. Comprising the following steps: 1) adding N-bromosuccinimide (NBS) into 4-iodobenzene serving as an initial raw material in an acetonitrile solvent in the presence of benzoyl peroxide serving as a catalyst, and reacting to obtain a 1-bromomethyl-4-iodobenzene compound II; 2) adding N-methylacetamide into the compound II in a tetrahydrofuran solvent by using potassium carbonate as alkali, and reacting to obtain an N-(4-iodobenzyl)-N-methylacetamide compound III; and 3) heating the compound III in a sodium hydroxide solution for deacetylation to obtain the compound IN-methyl-1-(4-iodophenyl) methylamine. The invention aims to provide a preparation process of the N-methyl-1-(4-iodophenyl) methylamine compound I, which is simple, convenient, green, environment-friendly and suitable for industrial production.

The utility model discloses an impurity removal reaction separation device for deuterated iodobenzene. The impurity removal reaction separation device comprises a reactor body and a separation assembly, the reactor body is provided with a concentrated hydrochloric acid inlet and a deuterated iodobenzene raw material inlet which are respectively used for introducing concentrated hydrochloric acid and deuterated iodobenzene into the reactor body; a plurality of iron balls are arranged in the reactor body, and the reactor body is heated through an oil bath; the deuterated iodobenzene raw materials comprise deuterated iodobenzene and deuterated nitrobenzene; the deuterated nitrobenzene can react with iron balls and concentrated hydrochloric acid in the reactor body in an oil bath heating environment to generate deuterated aniline, and the deuterated aniline generates water-soluble aniline hydrochloride under an acidic condition; the separation assembly is communicated with the reactor body and is used for separating water-soluble aniline hydrochloride and water-insoluble deuterated iodobenzene, so that impurity removal of deuterated iodobenzene is realized. According to the utility model, deuterated nitrobenzene in impurities can be removed, and high-purity deuterated iodobenzene can be obtained.

The present application relates to the field of organic synthesis, specifically a method for synthesizing C3 fluorine alkyl substituted quinoxaline ketone derivatives from olefin derivatives and quinoxaline ketone derivatives under photocatalysis by using [bis(fluoroalkyl acetoxy)iodo] benzene as different fluorine alkyl sources. [Bis(fluoroalkyl acetoxy)iodo] benzene is used as a fluorine alkylating agent to generate fluorine alkyl radicals under photocatalysis, then the radicals add to olefin derivatives to obtain alkyl radicals, the alkyl radicals then add to quinoxaline ketone, and finally, after oxidation and deprotonation, C3 fluorine alkyl substituted quinoxaline ketone derivatives are obtained. The present application uses simple and stable [bis(fluoroalkyl acetoxy)iodo] benzene as a fluorine alkyl source to prepare C3 different fluorine alkyl substituted quinoxaline ketone derivatives from quinoxaline ketone and olefin derivatives in a three-component reaction without the action of photocatalysts. The synthesis method is simple and easy to operate, and different fluorine alkyl group substituted quinoxaline ketone derivatives can be quickly obtained.

This invention provides a method for the diarylation of C(sp3)-H bonds. The method comprises: reacting a pyridine derivative with pinacol iodophenylboronic acid in a catalytic system of Ag2CO3, an amino acid ligand, and a noble metal catalyst. This method can achieve highly efficient diarylation of distal methyl C(sp3)-H bonds with yields of 52-66%, under mild reaction conditions, and with simple operation.

The invention discloses a synthesis method of a benzomorpholone derivative, and belongs to the technical field of organic chemistry. According to the method, a 3-hydroxy-2-indolone derivative and a triazole derivative react in an organic solvent at the temperature of 20-30 DEG C by taking commercialized cheap iodobenzene as a catalyst and selecting a fluorine reagent as an oxidizing agent, so that the benzomorpholone derivative can be obtained. The method is simple to operate, the raw materials are easy to obtain, the reaction steps are short and efficient, and the reaction yield is as high as 96%.

The invention discloses a synthesis method of 2, 3, 5, 6-tetrachloropyridine, which is characterized in that pyridine is used as an initial raw material, dichloro iodobenzene is used as a chlorination reagent, MOF-Cu / Al is used as a synergistic catalyst, and 2, 3, 5, 6-tetrachloropyridine is prepared through reaction in an organic solvent. According to the present invention, the process conditions are mild, the operation is simple and convenient, the 2, 3, 5 and 6 sites of the pyridine ring can be efficiently and selectively chlorinated under the mild conditions, the yield is stabilized at 90% or more, the by-product iodobenzene can be recycled, and the generation of the HCl waste gas and the large amount of the solid waste in the traditional process is avoided.

The present application provides a preparation method of a carbazole-based organic electroluminescent host material. Using inexpensive substrates 2-bromo-5-fluoro-nitrobenzene and 1-naphthylboronic acid, the coupling intermediate S1 is obtained through a Suzuki coupling reaction, and the ring-closing intermediate S2 is obtained by reduction with triphenylphosphine; the brominated product S3 is obtained by reacting with a brominating reagent in a suitable solvent; the intermediate S4 is synthesized using iodobenzene or an iodobenzene derivative; the intermediate S5 is obtained by reacting an arylamine with intermediate 4; the ring closure is achieved through C-H activation under Pd catalysis to obtain the intermediate S6; the 7,9-dihydrobenzo[g]indolo[2,3-b]carbazole derivative S7 is synthesized using iodobenzene or a benzene derivative.

The present invention proposes a method for synthesizing 6H-benzo[c]chromen-6-one, which belongs to the field of organic synthesis technology. Benzoic acid and iodobenzene are reacted to prepare 6H-benzo[c]chromen-6-one. The present invention starts from benzoic acid, first undergoes an arylation reaction with iodobenzene, and after obtaining the important reaction intermediate 2-arylbenzoic acid, continues to undergo an intramolecular cyclization reaction. A catalyst, an oxidant, an additive, and a solvent are added to a reactor, and the reaction is started. After the reaction is completed, the target product is purified by column chromatography or recrystallization to obtain the target product. Compared with the prior art, the present invention has the advantages of simple reaction operation, short steps, and low cost.

The invention discloses a preparation method and application of a benzyl indolyl diphenylphosphine derivative, the structural general formula of the benzyl indolyl diphenylphosphine derivative is shown as follows: the benzyl indolyl diphenylphosphine derivative is obtained by using iodobenzene to initiate a free radical mediated anion transfer phosphorylation process; the compound is applied to the aspect of inhibiting kiwifruit canker pathogen and rice bacterial blight pathogen. Compared with the prior art, the benzyl indolyl diphenylphosphine derivative has obvious beneficial effects, the synthesized benzyl indolyl diphenylphosphine derivative is not disclosed, and part of compounds have certain bacteriostatic activity.

The invention belongs to the field of organic synthesis, and particularly relates to a synthesis method of diaryl compounds containing silicon atoms. Toluene as shown in a formula 1a, iodobenzene as shown in a formula 2a and vinyl silane as shown in a formula 3 are mixed to react in the presence of a catalytic amount of PdCl2 (dppf), phosphorus ligand 4, 6-di (diphenylphosphine) phenazine and alkali metals LiN (SiMe3) 2 and CsF, and the diaryl compound containing silicon atoms as shown in a formula 4 is synthesized through the reaction. According to the invention, the combination reaction of toluene, iodobenzene and vinyl silane is realized by adopting a catalytic amount of PdCl2 (dppf), and the palladium catalyst shows obvious catalytic performance.

This invention provides a palladium-catalyzed method for the decarbonylation and cyclization of o-halobenzoic esters to synthesize 1-substituted phenanthrene compounds. The method involves the decarbonylation and cyclization of o-substituted iodobenzene, norbornadiene, and o-halobenzoic esters in an aprotic solvent under palladium catalysis to yield 1-substituted phenanthrene compounds. This method uses o-halobenzoic esters as cyclizing agents, which not only expands the applicability of cyclizing agents but also offers advantages such as milder reaction conditions, no need for inert gas protection (e.g., nitrogen), and no use of organophosphorus ligands. It is an economical and convenient method for preparing 1-substituted phenanthrene compounds.

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 thiophenylalanine and a synthesis method and application thereof, the structural formula of thiophenylalanine is shown in the specification, in the structural formula, S atom substitutes any position of ortho-position, meta-position and para-position on phenylalanine benzene ring, R1 is an amino protecting group, R2 is H or C1-C10 alkyl, and R3 is Trt or tBu. The synthesis method comprises the following steps: weighing iodo-phenylalanine and mercaptan, adding a catalyst, alkali and a solvent, reacting at room temperature under the protection of an inert atmosphere, and after the reaction is finished, carrying out acid pickling, extraction, drying, concentration and column chromatography separation to obtain thio-phenylalanine. The synthesized thiophenylalanine is rich and diversified in structure and is more suitable for amino acid condensation. The synthesis method is simple and convenient to operate, rapid and efficient, and a target product can be obtained with excellent separation yield. The thiophenylalanine with various structures is suitable for synthesis of polypeptide molecules or biomacromolecules, and has important research value and application potential in the fields of chemical synthesis, drug research and development, life science and the like.

The invention belongs to the technical field of organic electrochemical synthesis, and relates to an electro-catalysis olefin diazotization reaction method, and belongs to the technical field of organic synthesis. Comprising the following steps: (1) adding an olefin compound, an azide source, a supporting electrolyte, an additive, an iodobenzene electrocatalyst and a solvent into a reactor; (2) inserting an anode and a cathode, and controlling current to carry out electro-catalytic reaction; and (3) after the reaction is finished, extracting and purifying to obtain a target product. The method for realizing the iodobenzene-mediated olefin diazotization reaction by using the two-phase electrochemical reaction system disclosed by the invention obtains olefin compound diazotization products with various substituent groups, and has the advantages of mild conditions, simplicity in operation, only addition of a catalytic amount of electrocatalyst, safety, greenness, low cost and wide variety universality of olefin substrates.

This invention discloses a covalent organic polymer (COP) supported palladium nanoparticle catalyst with adjustable bipyridine content, its preparation method, and its application in C-C bond coupling reactions. This invention prepares a COP support with a gradient of bipyridine content by controlling the mixing ratio of monomers 5,5'-diamino-2,2'-bipyridine and benzidine with 1,3,5-tris(p-formylphenyl)benzene. Utilizing the strong coordination of the nitrogen atom in the bipyridine unit with palladium, efficient palladium loading and high dispersion are achieved, yielding a series of Pd@COP heterogeneous catalysts. This catalyst has a simple preparation process, low palladium loading, and controllable cost. It exhibits excellent catalytic activity and stability in the Sonogashira coupling reaction, with mild reaction conditions and high product yield, making it suitable for the efficient synthesis of diarylaceyne compounds. The bipyridine content of the catalyst support in this invention can be precisely controlled, and the palladium loading increases with the increase of bipyridine content. The palladium is uniformly dispersed on the surface of the support without obvious agglomeration. In the Sonogashira coupling reaction of iodobenzene and phenylacetylene, the separation yield can reach 93% under optimal conditions. The catalytic activity is not significantly affected by the palladium loading density, and it has good prospects for industrial application.

The present invention discloses a novel fluorescent probe based on triphenylamine, a preparation method and application thereof, and the preparation method comprises the following steps: S1. dissolving 4-methoxyaniline and 1-bromo-4-iodobenzene in solvent A, then adding copper iodide, 1,10-phenanthroline and potassium tert-butoxide to react to obtain compound 1; S2. dissolving compound 1 obtained by S1, (5-formylthiophene-2-yl)boric acid and anhydrous potassium carbonate in solvent B, then adding PdCl2 (dppf) to react to obtain compound 2; S3. dissolving compound 2 obtained by S2 and malononitrile in solvent C, then adding triethylamine to react to obtain a TPA-CN probe. The TPA-CN probe is used to monitor exogenous and endogenous SO2 and viscosity changes in living cells. The present invention can perform dual imaging of SO2 and viscosity in biological systems and food samples.

The invention provides a preparation method of a 2-methyl-3, 4-diphenyl-1-p-toluenesulfonyl-1, 2-dihydroquinoline derivative, and belongs to the technical field of heterocyclic compounds. The preparation method comprises the following steps: adding a palladium catalyst, alkali, N-(2-(cyclopropylphenylene methyl) phenyl)-4-methylbenzenesulfonamide and iodobenzene into an organic solvent, reacting at 80 DEG C for 12 hours, and performing post-treatment to obtain the 2-methyl-3, 4-diphenyl-1-p-toluenesulfonyl-1, 2-dihydroquinoline derivative. The preparation method has the advantages of simple operation, mild conditions, cheap and easily available initial raw materials, high reaction efficiency and wide application range of functional groups, and can realize one-step efficient and rapid synthesis of the 2-methyl-3, 4-diphenyl-1-tosyl-1, 2-dihydroquinoline derivative.

This invention discloses a method for preparing a diarylcarbazole material, relating to the field of organic light-emitting device technology. The method includes: obtaining intermediate A through a nitration reaction of 4-bromo-2-chloro-1-fluorobenzene; obtaining coupling intermediate B through a Suzuki coupling reaction of intermediate A and 1-naphthoboric acid; preparing intermediate C through a nitro cyclization reaction of intermediate B; coupling intermediate C with iodobenzene or iodobenzene derivative D to form intermediate E; preparing pinacol borate intermediate F using intermediate E; obtaining intermediate H through a Suzuki coupling reaction of intermediate F and o-bromoaniline or o-bromoaniline derivative G; cyclizing intermediate H under alkaline conditions to obtain intermediate I; and coupling intermediate I with a haloaryl derivative J to obtain the diarylcarbazole material. The preparation route provided by this invention has high reaction selectivity, produces a single product, has no obvious reaction defects, and avoids the problems of isomers in cyclization reactions and polybromination in bromination reactions.

The application belongs to the technical field of organic synthesis, and provides a synthesis method of diiodosilane. The synthesis method is carried out in a first reactor and a second reactor connected in series. In the first reactor, a first metal chloride, a solvent, dichlorodisilane (DCS) and iodobenzene are added to carry out a pre-reaction. After the pre-reaction, the solvent, DCS and iodobenzene are continuously fed into the first reactor. Meanwhile, the pre-reaction liquid in the first reactor is continuously fed into the second reactor containing a second metal chloride. The first reactor and the second reactor carry out reactions simultaneously. When the volume of the reaction liquid in the second reactor reaches a target liquid level, the reaction liquid in the second reactor is continuously produced and collected to realize continuous preparation of diiodosilane. The synthesis method provided by the application has high conversion rate of DCS.

The invention discloses a synthetic method of a compound containing cyclopropane. The synthetic method comprises the following specific steps: (1) dissolving raw materials of 1-bromo-2-fluoro-4-iodobenzene and boride of cyclopropane in a solvent to obtain a mixed solution; and (2) in an oxygen-free environment, adding a palladium catalyst, a ligand and alkali into the mixed solution, uniformly mixing, and reacting the reaction system at the temperature of 60-120 DEG C to obtain the target product 1-bromo-4-cyclopropyl-2-fluorobenzene. According to the synthesis method, the target product is obtained through one-step reaction, and operation is simple and convenient; the cost is low, and the method is environment-friendly; the yield of the purified target product after the reaction is high; and a wider application value is provided in the field of medical intermediates containing cyclopropane.

The invention discloses a preparation process of a high-thermal-conductivity low-expansion electronic-grade modified amine hardener, and belongs to the technical field of heat-conducting materials.According to the amine hardener, 1, 6-dibromo pyrene and nitrophenylboronic acid are subjected to Suzuki reaction and nitro ring closing to prepare a macrocyclic aromatic amine product B, and then 1-bromo-4-iodobenzene-mediated Buchwald-Harwig coupling is performed to obtain the high-thermal-conductivity low-expansion electronic-grade modified amine hardener. And connecting the product B with melamine to obtain the product. The plane rigidity of the main body macrocyclic aromatic amine inhibits the disordered conformation change of molecules at high temperature and reduces the phonon transfer loss; pi-Pi accumulation exists in a large-plane benzene ring to form high crystallinity, gaps can be reduced, and an efficient heat conduction channel can be constructed; the polyfunctionality-NH-bond and epoxy resin can form a three-dimensional cross-linked network, and a heat-conducting network penetrating through the whole body is formed so as to improve the heat-conducting property; thermal expansion is inhibited through cooperation of the rigid large ring pi-pi effect and the high crosslinking degree; and the polar-NH-bond also enhances the adhesive force of the packaging layer to the substrate through the hydrogen bond and the coordination bond of the metal substrate.

The invention discloses a synthesis process of dapagliflozin. The method comprises the following steps: (1) preparing a Grignard reagent THF solution of 1-chloro-2-(4-ethoxybenzyl)-4 iodobenzene; (2) preparing 2, 3, 4, 6-tetra-O-acetyl-alpha-D-glucopyranosyl bromide; (3) in the presence of a catalyst containing anhydrous cerium chloride and titanium tetraisopropoxide, carrying out coupled reaction on the Grignard reagent THF solution obtained in the step (1) and the 2, 3, 4, 6-tetra-O-acetyl-alpha-D-glucopyranose bromide obtained in the step (2) at the temperature of-15 to-10 DEG C to obtain an acetylated dapagliflozin intermediate; and (4) carrying out deprotection reaction on the acetylated dapagliflozin intermediate obtained in the step (3) to obtain the dapagliflozin. Under a composite catalytic system, the reaction shows excellent stereoselectivity, the required beta-configuration C-glycoside product is specifically generated, and the generation of by-products such as alpha-isomers and the like is effectively inhibited.

The application discloses a method for preparing aniline compounds by reducing nitrobenzene and selectively iodinating the aniline compounds, and belongs to the field of organic chemistry. a In the iodination reaction of the aniline compounds, ICl is selected as an iodinating reagent, and R a COOH is used as a reaction solvent, so that the iodination reaction of the aniline compounds has excellent selectivity, and 2-iodo-3-methyl-5-trifluoromethylaniline can be prepared in a high yield (more than 80% of liquid-phase yield). Meanwhile, in the method for preparing the aniline compounds by reducing nitrobenzene, hydrazine or hydrazine hydrate is used as a reducing agent, and a catalytic amount of Raney copper is used as a catalyst, so that a series of m-trifluoromethylaniline compounds can be prepared in a green, environment-friendly and efficient manner; wherein, the Raney copper only needs a catalytic amount, and still has catalytic activity after the reaction is completed, and can be recycled.