27 results about "Iodobenzene" patented technology

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 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 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 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.

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.

The invention belongs to the technical field of preparation of deuterated organic compounds, and particularly relates to a method for synthesizing deuterated iodobenzene by taking elemental iodine as a raw material, which comprises the following steps: reacting sodium chlorite as an oxidant and elemental iodine as an iodinating agent with deuterated benzene to prepare the deuterated iodobenzene. According to the method for synthesizing deuterated iodobenzene, the conversion rate of deuterated benzene with high price is increased, no by-product is generated, the requirement on equipment is low, heavy water or semi-deuterated water generated by reaction can be recycled, and the utilization rate of a deuterium source is increased.

The application relates to the technical field of organic silicon materials, in particular to a high-temperature-resistant coupling agent and application of the high-temperature-resistant coupling agent in a polyphenyl ether base material circuit board, wherein the high-temperature-resistant coupling agent has a structure shown in formula I. The high-temperature-resistant coupling agent is prepared by coupling reaction of an o-aminophenol compound and p-phenyloxy iodobenzene to obtain an intermediate, and then reacting the intermediate with chlorosilane in the presence of alkali. The high-temperature-resistant coupling agent contains an aromatic ring structure, a siloxane group and a polar adaptive site at the same time, has high matching degree with polyphenyl ether resin, benzoxazine resin, inorganic fillers and metal foils, can significantly improve the interface bonding force between copper foils and polyphenyl ether base materials, is synthesized by a two-step method, has mild reaction conditions, simple post-treatment, stable yield and less waste, and is suitable for large-scale industrial production.

This invention belongs to the field of molecular synthesis and materials technology, and discloses a method for preparing small molecule materials based on benzothiophene-benzodithiophene (DBDTT) and benzoselenophene-benzodiselenophene, as well as their applications. The method includes: using 1-chloro-2-iodobenzene or 1-chloro-2-bromobenzene and trimethylethynylsilane as raw materials, after a stalk coupling reaction, removing the TMS (trimethylsilyl group) with potassium hydrofluoric acid to obtain a key intermediate; using S8 or Se as a sulfur source or selenium source, and potassium carbonate as a base, a series of fused-ring thiophene / selenophene small molecule materials are synthesized through a cascade cyclization reaction. The substrates of this invention are simple to synthesize, the raw materials are inexpensive and readily available; no metals are involved; the reaction can be carried out under air conditions; the reaction efficiency is high, with three rings fused simultaneously in a single step; the yield is moderate, and even at a large scale (10 mmol), the yield can still reach 58%. Therefore, this method is suitable for industrial production.

The application discloses a preparation method of 3-hydroxy-2-indolone compounds. An o-iodo aryl alpha-ketoamide is reacted with sodium hydride in a solvent, the sodium hydride is activated and Na-I exchange reaction with iodobenzene occurs, and then intramolecular nucleophilic attack on the ketone carbonyl of the alpha-ketoamide is carried out, so that a series of 3-hydroxy-2-indolone derivatives which are difficult to synthesize by other methods are prepared. The method is simple in operation and mild in reaction condition, and does not need any transition metal catalyst, so that the method provides a new, direct and efficient synthesis strategy for preparing 3-hydroxy-2-indolone compounds. The method for preparing 3-hydroxy-2-indolone products has application value in drug synthesis.

The invention discloses a novel AIE photosensitizer as well as a preparation method and application thereof. The molecule takes triphenylamine as an electron-donating group and iodobenzoselenazole as an electron-withdrawing group, and is constructed through thiophene, benzothiadiazole or carbazole units. Researches show that DZTSe can efficiently generate type I and type II active oxygen, has low dark toxicity and good mitochondrial targeting ability, and is distributed in organelles such as endoplasmic reticulum, Golgi apparatus and the like. Under illumination, DZTSe induces pyroptosis by activating a caspase-1 / GSDMD pathway, releases DNA by damaging mitochondria, activates a cGAS-STING pathway, and promotes expression of type I interferon and inflammatory factors. Animal experiments show that DZTSe can significantly prolong the lifetime of mice with prostatic cancer, convert an immunosuppression microenvironment into an immune support state, and effectively inhibit primary and distal tumors.

The application belongs to the technical field of angiographic agents, and particularly relates to a kind of angiographic agents for corpses and a preparation method thereof. The angiographic agent for corpses comprises the following components in parts by mass: 20-35 parts of iodine-containing polymer, 30-50 parts of iodinated benzene ring compound, 90-150 parts of glycerol triacetate, 30-40 parts of dimer acid, and 600-800 parts of liquid paraffin. The iodine-containing polymer is obtained by copolymerization of (meth) acrylic acid C4-6 alkyl ester, polyethylene glycol bisacrylate and iodine-containing monomer, and the iodine-containing monomer is selected from at least one of 3-iodine-acrylic acid ethyl ester, 3-iodine-acrylic acid methyl ester and (meth) acrylic acid iodinated benzyl ester. The angiographic agent can achieve excellent angiographic effect on corpses, and can also achieve ideal angiographic effect for necropsy of corpses with long death time, thereby providing strong support for necropsy.

This invention discloses an axially chiral bipyridine ligand, its preparation method, and its uses. The axially chiral bipyridine ligand has the structure of general formula (Ⅰ): the axially chiral bipyridine ligand contains a binaphthalene structure, wherein part A is selected from A-1, A-2, or A-3; part B is a hydrogen atom or is the same as part A. The complex catalyst formed in situ in the reaction system of the axially chiral bipyridine ligand and copper salt in this invention exhibits high catalytic activity, good to excellent enantioselectivity, and good substrate universality in the asymmetric ring-opening iodination, thioesterification, and hydrolysis of cyclic diaryliodonium salts to synthesize highly optically pure, diverse substituted 1,1'-bi-2-iodobenzene compounds, 1,1'-bi-2'-iodo-2-thioester compounds, and 1,1'-bi-2'-iodo-2-phenol compounds, respectively, showing great promise for industrial applications. This invention belongs to the field of asymmetric synthetic chemistry.