22 results about "Iodination reaction" patented technology

The invention relates to the technical field of grease chemical industry, and discloses high-iodine oleic acid and a preparation method thereof.The preparation method comprises the steps that waste grease is pretreated; adding a polar modifier into supercritical CO2 to selectively extract oleic acid; adding a polar accelerant compound system into the supercritical system to carry out iodination reaction; refining and separating the product through pressure gradient; and establishing a circulating reiodination system, and returning medium and low iodination products to the iodination step for continuous reaction through a supercritical phase back-mixing technology and precise iodine source addition. According to the method, the oleic acid extraction selectivity coefficient is increased by 40-60% by introducing the polar modifier, the iodination reaction rate is increased by 50-80% through a polar accelerant compounding system, the total yield is increased to 75-85% from 60-70% through a circulating reiodination system, the product purity reaches 95-98%, high-value utilization of the waste grease is achieved, the production cost is greatly reduced by 40-60%, and the method is suitable for industrial production. No organic solvent is left, and the method is environment-friendly.

The application discloses a preparation method of iopromide and intermediates thereof, and particularly relates to the fields of organic synthesis and medicinal chemistry, and the preparation method route is as follows: a compound of formula I is subjected to chlorination reaction, acylation reaction, reduction reaction and iodination reaction to prepare a compound of formula V, and then iopromide is further prepared, the method can not only avoid the generation of diacylation by-products (formula 18), but also effectively reduce the generation of diiodo compounds (formula 24) in the preparation process, the intermediates are easy to separate and purify, and high-purity products can be obtained at a high yield.

The application discloses a preparation method of a key intermediate of a montelukast sodium side chain acid, belongs to the technical field of pharmaceutical intermediates, and relates to a key intermediate of a montelukast sodium side chain acid, i.e. 1-bromomethylcyclopropylacetonitrile, which is characterized by the preparation method of the 1-bromomethylcyclopropylacetonitrile. The preparation method is as follows: taking tribromoneopentyl alcohol as a starting material, and obtaining 1-bromomethylcyclopropylacetonitrile through a cyclization reaction, an iodination reaction and a cyano substitution reaction. The 1-bromomethylcyclopropylacetonitrile is prepared by using a brand-new synthesis process, starting from tribromoneopentyl alcohol, through a cyclization reaction, an iodination reaction and a cyano substitution reaction. The method solves the blank of the preparation method of 1-bromomethylcyclopropylacetonitrile in the prior art, and also solves the defects of a long reaction theoretical cycle and a low actual yield and a large amount of impurities in the reaction of preparing 1-bromomethylcyclopropylacetonitrile by first preparing 1-hydroxymethylcyclopropylacetonitrile and then reacting phosphorus tribromide with the 1-hydroxymethylcyclopropylacetonitrile.

The application relates to a symmetrical zwitterion salt containing a double-sulfonimide structure and a synthesis method and application, and comprises the following steps: adding imidazole, a first 3-chloropropane sulfonamide (trifluoromethylsulfonyl) imide salt and a first MOH into a first organic solvent, carrying out a single grafting reaction under anhydrous and anaerobic conditions, filtering, rotary evaporating and drying to obtain a first product; adding a second 3-chloropropane sulfonamide (trifluoromethylsulfonyl) imide salt and MI into a second organic solvent, carrying out iodination reaction, standing and centrifugal separation to obtain supernatant containing a second product; mixing the supernatant and the first product to carry out secondary grafting reaction, and carrying out post-treatment to obtain the symmetrical zwitterion salt containing the double-sulfonimide structure. In the symmetrical zwitterion salt, the propylsulfonamide (trifluoromethylsulfonyl) imide groups are connected on both sides of the delocalized N atom, which is more conducive to cation dissociation, and the imidazole is used as a central group, the reaction activity is stronger, the internal salt is easy to form, and the yield is improved.

The invention discloses a preparation method of iopromide and an intermediate thereof, and particularly relates to the field of organic synthesis and medicinal chemistry, the route of the preparation method is as follows: a compound of formula I is subjected to chlorination reaction, acylation reaction, reduction reaction and iodination reaction to prepare a compound of formula V, and then iopromide is further prepared. The method not only can avoid the generation of a diacylation by-product (formula 18), but also can effectively reduce the generation of a diiodo compound (formula 24) in the preparation process, the intermediate is easy to separate and purify, and a high-purity product can be obtained at a relatively high yield.

The invention relates to the technical field of chemical synthesis of pesticides, in particular to a preparation method of a key intermediate-3-iodine-5, 5-dimethyl-4, 5-dihydroisoxazole of a high-efficiency herbicide pyroxasulfone, which comprises the following steps: by taking glyoxylic acid and hydroxylamine hydrochloride as initial raw materials, carrying out oximation reaction to obtain glyoxylic acid oxime; then efficiently completing an iodination reaction through a potassium iodide / iodine elementary substance system under a mild condition, and controlling the reaction process to reduce the generation of byproducts so as to obtain high-purity diiodoformaldoxime; and finally, carrying out addition reaction with isobutene under the condition of normal pressure to finally obtain the target product with high purity and high yield. The core innovation point of the invention is to develop and verify multiple types of novel iodination catalysts, solve the problems of excessive iodine source, poor selectivity and long reaction period in the traditional iodination reaction, and realize collaborative improvement of reaction efficiency, selectivity and economy. The method has the characteristics of more efficient route, more controllable conditions, safer operation, further improvement of yield and purity, higher cost advantage and the like, and the industrial application value is remarkably enhanced.

The application discloses a preparation method of 2,2'-di(trifluoromethyl)-4,4',5,5'-biphenyl dianhydride, which comprises the following steps: ① iodization reaction of o-xylene to obtain 1,2-diiodo-4,5-xylene; ② coupling reaction of the product of step ① to obtain 2,2'-diiodo-4,4',5,5'-tetramethyl biphenyl; ③ trifluoromethylation of the product of step ② to obtain 2,2'-di(trifluoromethyl)-4,4',5,5'-tetramethyl biphenyl; ④ oxidation of the product of step ③ with an oxidant to obtain 2,2'-di(trifluoromethyl)-4,4',5,5'-biphenyl tetraacid; and ⑤ dehydration and cyclization of the product of step ④ to obtain 2,2'-di(trifluoromethyl)-4,4',5,5'-biphenyl dianhydride. The synthetic route provided by the application has the advantages of mild reaction condition, simple treatment, high efficiency and low cost.

This invention discloses an industrial production method for low-color 1,3-diiodo-5,5-dimethylhydantoin. It innovatively employs an integrated reaction system of "dual-catalyst synergy + microwave assistance + chlorine-oxygen composite oxidation." The synergistic effect of the dual catalysts reduces the activation energy of the iodination reaction and improves reaction selectivity. Furthermore, the non-thermal effect of microwaves accelerates the collision efficiency of reactant molecules. Simultaneously, oxygen partially replaces chlorine, reducing the formation of chlorinated impurities and shortening the reaction cycle. A post-processing technique of "gradient pH control + potassium iodate-ethanol composite rinsing + vacuum freeze-drying" is constructed. First, gradient pH adjustment promotes the crystallization of the target product. Then, the high solubility of ethanol for organic coloring impurities and the oxidation effect of potassium iodate on low-valent iodine impurities in the composite rinsing solution efficiently remove residual impurities. Combined with low-temperature freeze-drying, the product's color is prevented from changing color due to heat. Ultimately, the color of the product is stably controlled, extending its shelf life and meeting the stringent requirements of high-end medical and precision electronics fields for ultra-low color products.

The invention discloses a method for synthesizing a cefpodoxime proxetil intermediate 7-AMCA, and belongs to the technical field of cefpodoxime proxetil intermediate synthesis. The method is characterized in that a starting material D-7ACA is dissolved in a polar solvent liquid, and under the catalysis of an alkaline catalyst, elemental iodine is added to complete an iodination reaction, and then methanol is added to complete a methylation reaction to obtain a polar solvent liquid containing 7-AMCA. The method has the beneficial effects of using cesium acetate or cesium formate as an alkaline catalyst to carry out the methylation reaction, avoiding the use of reagents such as boron trifluoride and methanesulfonic acid, effectively reducing the risk factor, and the reaction reagents and solvents are non-highly toxic, and the harm to the environment and the human body can be almost ignored. The molar yield of the process can reach 85% or more, the product purity is 97.5% or more, and the by-product lactone is controlled to be below 0.3%.

The application discloses a novel method for preparing an intermediate of an aryl abietane diterpene Plebein C, and specifically comprises the following steps: substituting a carbonyl alpha position of 4,4-dimethyl-2-cyclohexen-1-ketone to obtain compound I; protecting the compound I by TBS to obtain compound II; performing a Luche reduction reaction on the compound II to obtain compound III; performing an iodination reaction on 3-hydroxy-4-methoxybenzaldehyde to obtain compound IV; performing a Wittig reaction on the compound IV to obtain compound V; performing a Mitsunobu reaction between the compound III and the compound V to obtain compound VI; performing a radical cyclization reaction on the compound VI to obtain compound VII; performing an oxidation on a benzyl position of the compound VII to obtain compound VIII; and finally performing an oxidation and a ring closure on the compound VIII to obtain a five-ring intermediate compound IX of a Plebein C molecule; the preparation method has the advantages of simple synthetic route, low-cost and easily-obtained reagents, high yield, favorability for industrial preparation of the intermediate, and strong popularization potential.

The invention provides a preparation method of an alkyl alcohol amine compound, which comprises the following steps: (1) mixing an alcohol compound with sodium iodide and zirconium chloride in a solvent, and reacting under a heating condition to obtain a reaction mixture containing an intermediate; and (2) mixing the reaction mixture with diethanol amine and an alkaline reagent, reacting under a heating condition, and purifying the obtained product to obtain the alkyl alcohol amine compound. According to the preparation method of the alkyl alcohol amine compound, the alcohol compound which is low in price and easy to obtain is adopted as the starting raw material, so that the raw material cost is remarkably reduced, and the economical efficiency of the synthesis process is improved. More importantly, a catalytic system consisting of zirconium chloride and sodium iodide is adopted to jointly act on the alcohol compound, so that efficient and high-selectivity iodination reaction is realized. The method has the advantages of mild reaction conditions, simple operation, simplified work flow, low toxicity and easy acquisition of raw materials, and easy purification of reaction products.

The invention discloses a photochemical synthesis method for high-selectivity conversion of an aromatic compound into aryl iodide, and belongs to the field of organic synthesis. The invention relates to a photochemical synthesis method for high-selectivity conversion of an aromatic compound into aryl iodide, which specifically comprises the following steps: in the absence of a solvent or an organic solvent, in the absence of an oxidant or in the presence of the oxidant, carrying out iodination reaction on the aromatic compound and an iodine elementary substance under visible light; and performing separation, purification, reduced pressure distillation or column chromatography purification to obtain the aryl iodide compound. The method provided by the invention is simple to operate, wide in application range and mild in reaction condition.

The invention belongs to the technical field of organic synthesis, and particularly discloses a preparation method and application of a polyiodo tetraphenylethylene derivative. Iodine atoms are introduced into para-positions of a plurality of benzene rings of a tetraphenyl ethylene skeleton, and at least one active group (carboxyl, nitryl, aldehyde group, hydroxyl, sulfydryl or amino) is accurately reserved. The preparation method comprises the following steps: by taking tetraphenylethylene with active group benzene ring para-substitution as a starting raw material, carrying out selective multi-site iodination reaction by adopting an iodination reagent under the catalysis of Lewis acid; and carrying out amidation reaction to realize derivatization of active groups. The technical contradiction that multi-site iodination and functional group retention are difficult to realize synchronously in the prior art is solved, and the obtained derivative has the characteristics of aggregation-induced emission, heavy atom effect, biological coupling activity and the like, and can be applied to the fields of biomedical imaging, medicine, chemical and biological sensing, organic synthesis, radiation detection, scintillation materials and the like. Wide application prospects are realized.

The invention relates to lignin developing microspheres as well as a preparation method and application thereof, and belongs to the technical field of embolism agents. The preparation method comprises the following steps: grafting N-hydroxyalkyl acrylamide on lignin to obtain modified lignin; mixing the modified lignin solution, an ionic monomer and an initiator in an aqueous solution to obtain an aqueous phase solution; adding the water-phase solution into the oil-phase solution to form a water-in-oil reversed-phase suspension polymerization system, and reacting to obtain lignin hydrogel microspheres; performing iodination reaction on the lignin hydrogel microspheres and iodine simple substances and / or iodine-containing compounds to obtain the lignin developing microspheres. The lignin developing microsphere has good X-ray developing performance, high strength and elasticity and good catheter passing ability, and the clinical application range of the developing embolism microsphere is widened.

According to the preparation method, sodium borohydride, iodine and a cyclic ether compound as shown in a formula I are taken as starting materials, dichloromethane is taken as a reaction solvent, metal cobalt salt is taken as a catalyst, and the ring-opening iodination reaction of the cyclic ether compound is realized under mild conditions, so that the diiodoalkane compound is prepared. And synthesizing the diiodoalkane compound (formula II). According to the method, a phosphorus-containing reagent does not need to participate, corrosion of an acid medium to reaction equipment is avoided, the used raw materials are wide in source and low in cost, aftertreatment operation is easy and convenient, safety and environment friendliness are achieved, the green chemical requirement is met, and the important practical value and the good application prospect are achieved.

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 discloses a compound TBFC-I as well as a preparation method and application thereof. The invention provides a novel compound TBFC-I. The novel compound TBFC-I has a chemical structural formula as shown in a formula II, and a preparation method of the novel compound TBFC-I comprises the following steps: in a carboxylic acid solvent, reacting 4-oxo-4, 5, 6, 7-tetrahydro-1-benzofuran-3-carboxylic acid (TBFC) with an N-iodoamide compound for 8-24 hours at the temperature of-5 DEG C to 30 DEG C, and carrying out electrophilic iodination reaction to generate iodinated TBFC, namely the compound TBFC-I. Compared with TBFC, the TBFC-I disclosed by the invention has the advantage that the inhibiting and preventing effects on plant disease pathogenic bacteria are obviously improved.

The invention discloses a synthetic method of a natural product Racemosin B, and belongs to the field of organic synthesis. The method comprises the following steps: by taking indole as a raw material, carrying out an iodination reaction and an N-H protection reaction to obtain an iodinated indole compound 2, then carrying out a coupling reaction on the iodinated indole compound 2 and methyl acrylate under the synergistic catalysis of palladium / norbornene to obtain a 2, 3 '-bisindole compound 3, and then carrying out a ring closing and deprotection one-pot reaction under an iodine-mediated illumination reaction to generate the racemosin B. The method has the advantages of easily available raw materials, low price, unique and novel route design, short steps, mild reaction conditions and simple operation.

The invention discloses an iodinated flavone derivative electrochemical synthesis method, which comprises: adding a flavone derivative, potassium iodide and a solvent into an unseparated electrolytic bath, using a graphite rod as an anode and a platinum sheet as a cathode, stirring under the current condition of 10 milliamperes, and separating and purifying a reaction crude product to obtain the iodinated flavone derivative. The invention develops an electrochemical C-H iodination reaction of potassium iodide and flavone derivatives, a series of functionalized iodinated flavone derivatives can be constructed through simple operation, and compared with the traditional synthesis method, the method has the main advantages that: 1) the reaction condition is mild, and the reaction can be smoothly carried out at room temperature; the method has the advantages of simple operation, no need of nitrogen protection, no use of a chemical oxidant due to the fact that an electric oxidation method is used in the reaction, good tolerance of functional groups, high yield and short reaction time.

The invention is applicable to the technical field of organic chemistry, and provides a method for synthesizing tetra-substituted olefin by carbon iodination of nickel-catalyzed alkyne, which comprises the following steps: dissolving asymmetric internal alkyne, aryl iodide, a nickel catalyst, a ligand, alkali, a boron reagent and an additive in an organic solvent to carry out trans-carbon iodination reaction of alkyne in a water-free and oxygen-free nitrogen atmosphere to obtain tetra-substituted olefin. And separating and purifying to obtain a trans-olefin product. According to the present invention, the cheap metal nickel catalyst is combined with the boron reagent to achieve the alkyne single selective synthesis of the tetra-substituted olefin, the reaction system has characteristics of good chemical selectivity, mild condition and high yield, the double conversion modules can achieve the configuration-maintained tetra-substituted olefin conversion, and the high synthesis application value is provided; the stereoselectivity and regioselectivity are good (as high as E: Zgt; 99 / : 1, rrgt; 20: 1), excellent functional group tolerance is achieved, and the highest yield can reach 90%.

The application discloses a synthesis method of 3,6-di(trifluoromethyl)-pyromellitic dianhydride. The synthesis method comprises the following steps: 1,2,4,5-tetramethylbenzene is subjected to iodization reaction in the presence of iodine, persulfate, concentrated sulfuric acid and acetic acid to obtain 3,6-diiodotetramethylbenzene; 3,6-diiodotetramethylbenzene is subjected to trifluoromethylation reaction with TMSCF3 (trifluoromethyltrimethylsilane) in the presence of CuX and MF in a polar solvent to obtain 3,6-di(trifluoromethyl)-tetramethylbenzene; 3,6-diiodotetramethylbenzene and an oxidant are subjected to oxidation reaction to obtain 3,6-di(trifluoromethyl)-pyromellitic acid; and 3,6-di(trifluoromethyl)-pyromellitic acid is subjected to dehydration and cyclization with acetic anhydride to obtain 3,6-di(trifluoromethyl)-pyromellitic dianhydrate. The reaction condition of the application is relatively mild, the treatment is simple, the efficiency is relatively high, and the cost is relatively low.

The application provides a preparation method of methyl o-iodobenzoate. In the acid condition, methyl o-aminobenzoate is used as raw material, and nitroso sulfuric acid is added to generate iodination reaction to generate methyl o-iodobenzoate. The raw material methyl o-aminobenzoate is widely sourced and low in price. The reagents used in the whole preparation process are easy to obtain, the production cost is low, and the reagents are basically non-toxic and harmful. In the reaction process, the reaction condition is mild, the operation process is simple, the operation safety is high, the post-treatment is simple, a large amount of waste water is not generated, and the environment protection is beneficial. The prepared product is low in salt content and high in purity.