36 results about "O-iodoaniline" patented technology

The invention discloses a preparation method of a 2-trifluoromethyl substituted quinazolinone derivative, which comprises the following steps of: adding a palladium catalyst, a ligand, a carbon monoxide substitute, an additive, trifluoroethyl imine acyl chloride and o-iodobenzidine into an organic solvent, reacting at 90 DEG C for 16-30 hours, and after the reaction is completed, carrying out post-treatment to obtain the 2-trifluoromethyl substituted quinazolinone derivative. The preparation method has the advantages of simple operation, cheap and easily available reaction starting raw materials, compatibility with a plurality of substituents, good substrate applicability, realization of synthesis of trifluoromethyl quinazolinone derivatives substituted by different groups through substrate design, convenience in operation, and higher practicality. According to the method, 1, 3, 5-triformic acid phenol ester is used as a solid carbon monoxide substitute, so that the use of toxic and colorless gas carbon monoxide is avoided.

The invention relates to a synthesis method of tris-(4-tetrazolyl-phenyl)amine, belonging to the field of material chemistry. The technical scheme of the invention is as follows: reacting diphenylamine with halo-benzene under a basic condition to obtain triphenylamine, carrying out substitution reaction on triphenylamine with iodine to generate tris-(4-iodophenyl)amine, then reacting tris-(4-iodophenyl)amine with CuCN to generate tris-(4-cyanophenyl)amine, and finally reacting tris-(4-cyanophenyl)amine with sodium azide to generate tris-(4-tetrazolyl-phenyl)amine. The porous material built by reacting obtained tris-(4-tetrazolyl-phenyl)amine with a metal has the stability of carboxylic acid porous frames, achieves intra-pore functionalization, and has pores in a mesoporous size. The adsorption capacity with respect to specific sulfur-containing small molecules shows that the porous material has potential application value in developing high-performance petrochemical products.

The invention relates to a beta-naphthyl methyl substituted spiral bisoxazoline ligand, a synthetic method and an application. The ligand has the advantages of simple synthetic method, mild conditionand applicability for industrialization production. The ligand has a spiral framework and a feature of a plurality of chiral centers, therefore the ligand has high catalytic activity and chiral induction effect and strong adjustment capacity in an asymmetric catalytic reaction of transition metals. Pyrrolidine derivants with various optical activities are prepared through high region selectivity and high enantioselectivity from allenoic and o-iodoaniline by the catalysis of the ligand. With the important biological activity, the pyrrolidine derivant has a better prospect of industry and medicine applications.

The invention discloses a benzoselenazole compound as well as a preparation method and application thereof and belongs to the technical field of medicines. The preparation method of the benzoselenazole compound is characterized by preparing a series of methoxy-containing benzoselenazole compounds from o-iodoaniline derivatives, benzaldehyde derivatives and selenium under catalysis of copper through a one-pot process, and finally carrying out boron tribromide demethylation to obtain a hydroxy-containing benzoselenazole compound. In-vitro experiments show that the benzoselenazole compound as a ligand of an oestrogen receptor ER beta shows excellent agonist effect; the correlation research shows that the compound as an ERb ligand has treatment effect in animal model of rheumatic arthritis andintestinal diseases caused by inflammation, so that the benzoselenazole compound has potential treatment effect in treatment of rheumatic arthritis and intestinal diseases.

A preparation method of boscalid comprises following steps: o-iodoaniline and 2-chloronicotinyl chloride have a condensation reaction to produce an intermediate product 2-chloro-N-(2-iodophenyl)pyridine-3-formamide;2-chloro-N-(2-iodophenyl)pyridine-3-formamide which is not purified has a Suzuki coupling reaction with 4-chlorophenylboronic acid directly, and boscalid is produced. A Ni / C preparation method is provided, and Ni / C is taken as a catalyst for the Suzuki coupling reaction, so that the production cost is greatly reduced; further, production raw materials are available, the yield is high, and the preparation method of boscalid is applicable to large-scale industrial production.

The invention relates to a method for synthesizing 2-substituted benzothiazole by a one-pot method. The preparation method comprises the following specific steps: dissolving a 2-Iodoaniline compound,a styrene compound, elemental sulfur, an alkaline medium, a catalyst and a ligand in an organic solvent, and stirring for 10-24 hours at 100-140 DEG C to react to obtain 2-substituted benzothiazole; wherein the molar ratio of the 2-Iodoaniline compound to the styrene compound is 1: (1-3); and cooling, extracting, drying and column chromatography separation are carried out to obtain a pure product.The method has the advantages that (1) the reaction conditions are mild, the reaction activity is high, the reaction yield is high, the product selectivity is high, and the substrate expansion rangeis wide; (2) use of a large amount of solvents and noble metal compounds in a catalyst system is avoided, cost is low, the method is safe and convenient, and low environmental pollution is caused by the reaction system; and (3) no mixed solvent or oxygen is used in the reaction system, so that potential risks existing in oxygen use are avoided, and a reference value is provided for industrial application.

The invention discloses a preparation method of boron-containing indolinone derivatives, in particular to a method for synthesizing boron-containing indolinone derivatives through the cyclization reaction of copper-catalyzed o-iodoaniline derivatives and biboronic acid pinacol esters , belongs to the field of organic synthesis. The method uses o-iodoaniline derivatives and biboronic acid pinacol ester as raw materials, and under the catalysis of copper catalyst, through the joint action of ligands and basic compounds, in an organic solvent, the reaction is carried out at a temperature of 40-140° C. , and the boron-containing indolinone derivatives are obtained after post-treatment after the reaction. The invention uses easily prepared o-iodoaniline derivatives and commercially available pinacol esters as raw materials, and realizes the rapid construction of boron-containing indolinone derivatives by constructing one ring and two chemical bonds in one step. The reaction conditions are mild, the operation is simple, and the reaction raw materials are readily available, the substrates are widely applicable, and the target products are easily separated.

The invention discloses a polyquinazoline compound and its preparation method and application. The preparation method comprises the following steps: under the action of a catalyst and an alkali Multi-component polymerization reaction to obtain polyquinazoline compounds. The method of the invention has mild conditions, and the polymerization monomer is simple and easy to obtain. The polyquinazoline compound obtained in the invention has better solubility, processability and higher thermal stability, and has potential applications in the fields of metal ion detection and self-assembly.

The invention discloses a preparation method of a substituted 2,3-dihydroquinolone compound, comprising the following steps: adding a palladium catalyst, a ligand, a carbon monoxide substitute, an additive, N-pyridinesulfonyl-o-iodoaniline and an alkene into an organic In a solvent, the reaction is carried out at 100-120° C. for 24-48 hours. After the reaction is complete, post-treatment is performed to obtain the substituted 2,3-dihydroquinolone compound. The preparation method is simple to operate, the starting materials are cheap and easy to obtain, the reaction efficiency is high, and the substrate compatibility is good, and the 2,3-dihydroquinolone compound substituted by the 2-position aryl group and the 3-position alkyl group can also be synthesized through substrate design , which is easy to operate and broadens the practicability of this method.

The invention relates to the field of compound preparation, particularly a preparation method of a novel bactericide boscalid. The method comprises the following steps: in a polar aprotic solvent or high boiling solvent, carrying out Suzuki reaction on a palladium catalyst p-chlorophenylboric acid and o-acetaminobrombenzene in the presence of alkali and quaternary ammonium salt to obtain an intermediate product 4'-chloro-2-acetaminobiphenyl; and deprotecting the intermediate product in the presence of concentrated hydrochloric acid, and condensing with 2-chloronicotinoyl chloride. According to the method, the Pd(OH)2 / C is used as the catalyst to perform the Suzuki coupling reaction, and is recovered and reutilized many times; and thus, compared with the prior art, the method provided by the invention greatly saves the catalyst cost, is convenient for recovering the catalyst, and avoids using the high-cost raw material o-iodoaniline.

The invention discloses a method for melting, crystallizing, separating and purifying iodoaniline. The method comprises the following steps: 1) grinding an iodoaniline and paraiodoaniline mixture rawmaterial into powder to obtain a product A; 2) putting the product A into a crystallizer, starting the crystallizer, heating the product A and completely melting the product A to obtain a product B; 3) cooling the product B to perform crystallization, growing the crystal after the crystallization final temperature is arrived, and discharging mother liquid to obtain a product C; and 4) heating andsweating the product C step by step until the sweating final temperature and discharging the sweat, wherein the residual crystal is the purified iodoaniline. The method provided by the invention has the characteristics of no need of organic solvent, environmental friendliness, high separation and purification efficiency, small loss amount of iodoaniline, low cost and high purity of the iodoaniline, and is suitable for industrialized popularization.

A preparation method of boscalid comprises following steps: o-iodoaniline and 2-chloronicotinyl chloride have a condensation reaction to produce an intermediate product 2-chloro-N-(2-iodophenyl)pyridine-3-formamide;2-chloro-N-(2-iodophenyl)pyridine-3-formamide which is not purified has a Suzuki coupling reaction with 4-chlorophenylboronic acid directly, and boscalid is produced. A Ni / C preparation method is provided, and Ni / C is taken as a catalyst for the Suzuki coupling reaction, so that the production cost is greatly reduced; further, production raw materials are available, the yield is high, and the preparation method of boscalid is applicable to large-scale industrial production.

The invention discloses a fluorescent probe for identifying thiocyanate and its preparation and identification method. The molecular formula of the probe is C 57 h 75 Br 3 N 4 . Its preparation method is to first mix tris(4-iodophenyl)amine and 4-pyridine boronic acid, then be dissolved in the mixed solution of dioxane and water to obtain product A; product A is placed in a nitrogen-protected environment, Add Pd(PPh 3 ) 4 and Na 2 CO 3 , stirred at 80-100°C for 10-20h, cooled to 20-30°C after the end, diluted with water, and then extracted to obtain product B; with anhydrous Na 2 SO 4 Dry product B, then spin dry the solvent, and purify by column chromatography to obtain product C as a yellow solid; dissolve product C in N,N-dimethylformamide, then add bromooctane, heat to 75-85°C, After reacting for 30-40 hours, diethyl ether was added to the reaction solution until it was completely precipitated, filtered with suction, the solid was washed with diethyl ether, and dried to obtain a fluorescent probe for recognizing thiocyanate. The probe of the invention can identify thiocyanate, and has the characteristics of sensitive identification, high selectivity, simple operation, no pollution and low cost.

The invention relates to a beta-naphthyl methyl substituted spiral bisoxazoline ligand, a synthetic method and an application. The ligand has the advantages of simple synthetic method, mild condition and applicability for industrialization production. The ligand has a spiral framework and a feature of a plurality of chiral centers, therefore the ligand has high catalytic activity and chiral induction effect and strong adjustment capacity in an asymmetric catalytic reaction of transition metals. Pyrrolidine derivants with various optical activities are prepared through high region selectivity and high enantioselectivity from allenoic and o-iodoaniline by the catalysis of the ligand. With the important biological activity, the pyrrolidine derivant has a better prospect of industry and medicine applications.

The invention discloses synthesis methods of a rhazimine tetracyclic skeleton. One of the synthesis methods adopts the following linear synthesis route: gamma-hydroxy-alpha,beta-unsaturated ester having a [3,3,1] ring system structure is adopted an initial raw material; a methanol group protects the hydroxyl group of allyl alcohol, and deconjugation alkylation is creatively used to achieve the migration of a double bond and construct a whole carbon quaternary carbon center; lithium tetrafluoroborate undergoes silicon deprotection and alkenyl ether structure hydrolysis; an aldehydic carbonyl group obtained by oxidizing a primary alcohol and o-iodoaniline undergo reducing amination, and a ketocarbonyl group is reduced; a secondary alcohol is oxidized; and the rhazimine tetracyclic skeleton is constructed through the alpha-position coupling of the carbonyl group. The other one of the synthesis methods adopts the following convergent synthesis route: a methyl-protected allyl alcohol structure and chloride connected with the o-iodoanide fragment undergoes deconjugation alkylation, and then intramolecular coupling is carried out to construct the rhazimine tetracyclic skeleton. The synthesis methods have the advantages of simple operating steps, low requirements of reaction conditions, and high-efficiency synthesis of the target compound.

The invention discloses 9-aza-bicyclo[3.3.1] nonane coupled iodine-rich compounds. A preparation method of the compound comprises steps as follows: 9-nitrogen(6'-amino)hexylamine-9-9-aza-bicyclo[3.3.1] nonane-3 alpha-alkylamidophenyl formate and a chloroacetyl triiodoaniline derivative are mixed in an organic solvent in the mole ratio being 1:(1.0-1.5) and subjected to a reaction at the room temperature under the catalytic action of cesium hydroxide for 20-30 h, and a product, namely, the 9-aza-bicyclo[3.3.1] nonane coupled iodine-rich compounds, is obtained. The invention also discloses an application of the 9-aza-bicyclo[3.3.1] nonane coupled iodine-rich compounds as a contrast medium for early diagnosis of breast cancer.