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56 results about "Iodine catalysis" patented technology

Tiotropium bromide anhydride and preparation method thereof

The invention discloses a method for preparing tiotropium bromide anhydride, which comprises the steps of: under the anhydrous and anaerobic condition, preparing an intermediate I by taking a special kettle bottom valve and a multi-functional reaction kettle as a reactor, taking a special filter as refining equipment and taking hydrobromic scopolamine as an initial raw material through reduction hydrogenation reaction; preparing an intermediate II by performing addition reaction of Grignard reagent and dimethyl oxalate in tetrahydrofuran, wherein the Grignard reagent is prepared from bromothiophene by taking tetrahydrofuran as a medium through iodine catalysis; preparing an intermediate III by performing ester exchange condensation reaction of the intermediate I and the intermediate II under the action of sodium; preparing an intermediate IV from the intermediate III through methylation bromination reaction; and preparing the tiotropium bromide anhydride by performing the activated carbon decoloration and recrystallization on the intermediate IV by using aqueous solution and acetonitrile methanol isopropyl ether solution. Compared with those in the prior art, reaction products of the method have the advantages of good quality, high yield, controlled reaction process, safe production and good environmental protection effect.
Owner:HONGYI SCI & TECH CO LTD NANCHANG

Iodide ion detection reagent based on iodide catalyzed hydrazine-[oxidant-Ferroin reagent] and iodide ion detection method

The invention discloses an iodide ion detection reagent based on iodide catalyzed hydrazine-[oxidant-Ferroin reagent] and an iodide ion detection method. In an acid medium, a tetravalent cerium solution or potassium permanganate solution is used for oxidizing an orange red Ferroin reagent solution into a blue solution in an acid medium, and a hydrazine saline solution is added to enable the blue solution to generate a reaction that blue is slowly faded to be turned into orange red; iodine has a sensitive oxidizing effect for the reaction, the higher the iodine concentration is, the higher thereaction speed is, a proportional relation is formed between the iodine concentration and the luminance value, and the iodine content of a sample can be calculated by an iodine standard curve. The detection result can be consistent to the result of the iodine tested by adopting a classical arsenic-cerium catalytic photometric method, and the use of a virulent hard-to-purchase arsenic trioxide reagent in the classical arsenic-cerium catalytic photometric method is avoided. The detection method has the advantages of being simple and convenient, rapid, specific, sensitive, accurate and the like,is expected to be widely applied to related fields needing to detect the iodine content of the sample, and especially is applied to urine iodine and water iodine detection in the fields of sanitary inspection and medical technology.
Owner:XIAMEN CENT FOR DISEASE CONTROL & PREVENTION

Method for preparing acetylated hemicellulose by employing catalysis of iodine

The invention discloses a method of applying iodine catalysis to prepare for acetylated hemicellulose. Firstly, KOH solution is used to dispose delignified wheat straw, then, dissolved alkali-soluble hemicellulose in filtrate is processed for purification and separation; subsequently, the hemicellulose after separation is added into 1-butyl-3-methyl imidazole chloride solution, the catalyst iodine with the weight of corresponding 10 percent to 15 percent of the hemicellulose is added, then the acetic anhydride which is 16 to 28 times of xylan hydroxyl in the compositions of the hemicellulose is added to react for 20 to 30 minutes under 90 DEG C to 110 DEG C and cooled, saturated sodium thiosulfate is added into a mixture, and ethanol is used for washing and drying to obtain the acetylated hemicellulose. The invention can obtain the acetylated hemicellulose with high substitution degree; compared with a heterogeneous system, the invention improved the reaction speed by five to ten times, increases the output and reduces the production cost, the hydrophobic nature of the hemicellulose after chemical modification is improved greatly, and the invention can be used for preparing for the degradable food-packing film.
Owner:SOUTH CHINA UNIV OF TECH

Preparation method and application of azobenzene-based light energy storage phase change material

The invention discloses a preparation method of an azobenzene-based light energy storage phase change material. The method comprises the following steps that: (1) preparing photoresponse azobenzene molecules: carrying out a reaction on 4-hydroxyazobenzene and 1-bromoalkane by using N, N-dimethylformamide as a solvent under an alkali and iodine-containing catalyst condition to obtain 4-alkoxy azobenzene energy storage molecules; and (2) preparing the azobenzene light energy storage phase change material: carrying out melt blending on the 4-alkoxy azobenzene energy storage molecules prepared inthe step (1) and an organic phase change material, fully stirring the molecules and the organic phase change material to obtain the azobenzene light energy storage phase change material. The phase change point of the phase change material decreases under ultraviolet irradiation, the phase change point of the phase change material rises under visible light irradiation, light response phase change control exists. The azobenzene light energy storage molecules have photochromic performance; the change of the color can indicate the change of an isomerism degree; and based on the corresponding relation, an energy storage state can be monitored, and the utilization efficiency of energy is improved.
Owner:JIANGNAN UNIV

Dithiocarboxylic acid pentafluorobenzyl ester, preparation method and application thereof

The invention discloses a dithiocarboxylic acid pentafluorobenzyl ester, a preparation method and an application thereof. A structural formula of the dithiocarboxylic acid pentafluorobenzyl ester is shown in a specification, the preparation method comprises the following steps: taking pentafluoride bromo-carbons as a substrate, under iodine catalysis, reacting the substrate and magnesium powder or reacting the substrate and brominated ethyl magnesium for synthesizing a grignard reagent having a pentafiuorophenyl end group, reacting the reagent with carbon disulfide for synthesizing to obtain dithiocarboxylate, then performing an esterification reaction with alpha-bromine-2,3,4,5,6-pentafluorotoluene to prepare the dithiocarboxylic acid pentafluorobenzyl ester. According to the invention, the dithiocarboxylic acid pentafluorobenzyl ester can be taken as a high fluorine-containing RAFT reagent, can be used for a supercritical carbon dioxide system to realize RAFT polymerization of a (methyl) fluoroalkyl acrylate fluorine-containing monomer under mild condition, and the prepared fluorine-containing polymer having a highly stable pentafiuorophenyl end group. The polymer has good hydrophobicity, weatherability and soiling resistance, the high fluorine-containing end group can enhance heat stability and transmittance of the polymer, so that application requirement under special condition can be satisfied.
Owner:SHAANXI NORMAL UNIV

Method for synthesizing 1,2,3-triaryl-1-acetone compound from benzyl chloride through non-metal-catalyzed carbonylation

The invention discloses a method for synthesizing a 1,2,3-triaryl-1-acetone compound from benzyl chloride through non-metal-catalyzed carbonylation. According to the method, carbon monoxide is taken as a carbonyl source, and an iodine catalyst is utilized for catalyzing carbonylation-alkylation domino reaction of benzyl chloride and an aryl boron reagent in medium polyethylene glycol in the presence of the iodine catalyst and alkali so as to directly prepare the 1,2,3-triaryl-1-acetone compound. In the method, noble metal catalysts and ligands are not used, and the reaction can be carried out under the normal pressure; and the method has the advantages that a substrate is wide in source, stable and low in cost, the catalyst is low in cost and easily available, little waste is produced, the application range is wide, the reaction selectivity is high, and the yield of the target product is high.
Owner:NANJING NORMAL UNIVERSITY

Method for preparing cyanophenyl compound

The invention relates to a method for preparing a cyanophenyl compound, which comprises the following steps: adding an alkoxy benzene compound, iodine, catalyst copper nitrate, cyanide and an acetonitrile solvent into a reaction vessel in sequence, wherein the weigh ratio of the alkoxy benzene compound to the cyanide, the catalyst copper nitrate and the iodine is 1:(0.1-5):(0.8-1.2):(0.4-0.5), then sealing the reaction container, agitating and reacting for 5-45 hours at a temperature of 150-200 DEG C, cooling to a room temperature after reaction and purifying a reacted mixture through a column chromatography to obtain the cyanophenyl compound. The preparation method has the beneficial effects that the relatively-cheap the alkoxy benzene compound is taken as a raw material, acid and high-pressure gas are not used, the production cost is remarkably reduced, and as low-boiling point solvent acetonitrile is used, a product is easy to separate and purify.
Owner:HENAN UNIV OF SCI & TECH

Regioselective deoxidation thionation reaction for 7-azaindole-nitrogen oxide

InactiveCN110759907AEasy to operateRegioselective regulationOrganic chemistryPtru catalystOrganic synthesis
The invention relates to the fields of organic synthesis and medicine and chemical industry, in particular relates to an iodine-catalyzed regioselective deoxidation thionation reaction method for 7-azaindole-nitrogen oxide, and aims to overcome the problems of high toxicity, low efficiency and poor adaptability existing in the prior art. The technical solution adopted in the invention is characterized in that the method comprises the following steps: by using the 7-azaindole-nitrogen oxide as a substrate and an internal oxidant, and a disulfide as a thioetherification reagent, under the condition of the molar ratio of the 7-azaindole-nitrogen oxide to the disulfide of 1:(0.5-2), adding molecular iodine as a catalyst, and performing a deoxidation thioetherification reaction in a solvent, wherein the use amount of the solvent is 2-10 mL, and the molar concentration of the 7-azaindole-nitrogen oxide is 0.1-0.5 mol / L; and sequentially adding the measured reactants into a pressure-resistanttube with a magneton, sealing the pressure-resistant tube, performing stirring on a magnetic stirrer at room temperature, performing a reaction at pressure of 0.1 MPa and temperature of 80-120 DEG Cfor 12-36 h, performing cooling to room temperature, performing extraction for several times, combining organic phases, removing the solvent, and performing purification to obtain 7-azaindole sulfide.
Owner:SHAANXI UNIV OF SCI & TECH

Indole heterocyclic compound, preparation method thereof and application of indole heterocyclic compound in prevention and treatment of plant diseases

The invention discloses an indole heterocyclic compound as well as a preparation method and application thereof in prevention and treatment of plant diseases. According to the method, indole is reacted with oxalyl chloride to obtain indole oxalyl chloride, then indole oxalyl chloride is reduced by tributylstannane to obtain indole carbonyl acetaldehyde, and finally indole carbonyl acetaldehyde isreacted with a corresponding amino acid under the catalysis of iodine to obtain a compound. The indole heterocyclic compound provided by the invention shows especially excellent plant virus resistingactivity, can well inhibit the tobacco mosaic virus, and also shows broad-spectrum plant pathogenic bacteria resisting activity.
Owner:TIANJIN NORMAL UNIVERSITY

Production process of high-purity aminoacetaldehyde dimethyl acetal

The invention discloses a production process of high-purity aminoacetaldehyde dimethyl acetal. The process comprises the following steps: proportionally mixing chloroacetaldehyde dimethyl acetal withanhydrous liquid ammonia to react, and carrying out ammoniation, deamination recovery, alkali neutralization desalination, distillation and rectification in the presence of an iodine-containing catalyst to obtain the high-purity aminoacetaldehyde dimethyl acetal. According to the method, chloroacetaldehyde dimethyl acetal is innovatively used as a main raw material, anhydrous liquid ammonia is used as a solvent and a reaction raw material, an iodine-containing catalyst is added, and the anhydrous high-purity aminoacetaldehyde dimethyl acetal is obtained through ammoniation, deamination, alkalineutralization desalination, distillation and rectification. In practice, the technical process can reduce the generation of by-product conjugates, can realize higher conversion rate than the traditional process under the condition of higher catalytic effect, and simultaneously reduces the requirements on organic solvents and energy sources; and under the condition of the same proportion, the single-batch feeding amount and the product yield of the novel process are improved by 50% or above, the yield is about 20% higher than that of a traditional process, and the effects of saving energy, improving quality, reducing cost and reducing consumption can be achieved.
Owner:INNER MONGOLIA SAINTCHEM CHEM

Synthesis technology of benthiavalicarb isopropyl

The invention discloses a new synthesis technology of benthiavalicarb isopropyl, and belongs to the field of pesticide chemistry. A method for implementing the synthesis technology comprises the steps as follows: fluorocyclohexanone is used as a raw material and catalyzed by iodine to generate 2-amino-6-fluorobenzothiazole through oxidative cyclization, and after hydrolysis and acidification, 2-amino-5-fluorothiophenol is prepared; meanwhile, D-alanine is used as a raw material and reacts with triphosgene to generate (R)-4-methyl-oxazolidine-2, 5-diketone, and an intermediate reacts with 2-amino-5-fluorothiophenol to prepare chiral (R)-1-(6-fluorine-benzothiazole-2-) ethylamine; and L-valine is used as a raw material and reacts with isopropyl chlorocarbonate to prepare N- Isopropoxy carbonyl-L-valine, carboxyl activation is performed simultaneously, and finally, the raw materials and (R)-1-(6-fluorine-benzothiazole-2-) ethylamine perform a one-pot reaction to directly generate benthiavalicarb isopropyl. The synthesis technology has short process route and high total yield, and purity degree is higher than 95%.
Owner:SHANGQIU NORMAL UNIVERSITY

Reagent and method for detecting iodine through antimony-cerium reaction iodine catalysis method

A classic trace iodine detection method is an arsenic-cerium catalytic spectrophotometric method, such as a sanitary industry standard method WS / T 107-2016 for urine iodine detection, and is widely applied to iodine deficiency and iodine nutrition monitoring in China. However, a highly toxic arsenic trioxide (arsenic trioxide) reagent needs to be used in the method, and the application of the method is increasingly limited due to environmental protection. A non-toxic trace iodine detection reagent and a non-toxic trace iodine detection method are urgently needed in the field of health care. The invention discloses a reagent and a method for detecting iodide ions by adopting an iodine catalyzed antimony-cerium redox reaction principle. Iodine ions catalyze Sb < 3 + > to reduce yellow Ce < 4+ > into colorless Ce < 3 + >, and the reaction speed and the iodine content are in a positive correlation quantitative relation. And after a certain reaction time, the absorbance of the residual Ce< 4 + > in the solution is measured by using a spectrophotometric method, and the iodine content of the measured sample is calculated according to the quantitative relationship between the iodine content and the absorbance. According to the method, toxic-free antimony is adopted to replace highly-toxic arsenic in a classic method, the detection effect consistent with that of an arsenic-cerium catalytic spectrophotometry is achieved, the highly-toxic arsenic trioxide reagent is prevented from being used, and the method is applied to detection of urine iodine, blood iodine, water iodine, salt iodine, food iodine, soil iodine and the like and has important public health significance.
Owner:刘列钧

Method for preparing bromoacetonitrile from chloroacetonitrile

The invention discloses a method for preparing bromoacetonitrile from chloroacetonitrile, and belongs to the field of chemical engineering. The method comprises the following steps: heating and refluxing chloroacetonitrile, inorganic bromide and an iodine-containing catalyst in a solvent, and purifying after the reaction is completed to obtain bromoacetonitrile. The easily available inorganic bromide is used as the bromine source, the used solvent is environment-friendly and recyclable, the reaction yield is greatly improved, the post-treatment method is simple, and the whole reaction route is clean and environment-friendly.
Owner:沧州维智达美制药有限公司
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