133 results about "Iodination reaction" patented technology

The invention relates to a synthetic method of ceftazidime intermediate; 7-amino cephalsporanic acid is used as a raw material; a silanization reaction, an iodination reaction, and a pyridine reaction are performed; the obtained product is added with an oxidant, and hydrochloric acid or is added into a mixed solvent of an organic solvent and water to prepare a halogen acid salt of the ceftazidimeintermediate (6R, 7R)-7-amino-3-pyridine methyl-ceph-3-ene-4-carboxylic acid. The invention also provides a method for preparing ceftazidime by using the obtained intermediate halogen acid salt. The ceftazidime intermediate and ceftazidime prepared by the methods have high yield, and low production cost; the operation is simple; the discharge of three wastes is less; treatment and recovery are easy, and the methods are applicable to industrial production.

The invention discloses an improved method for preparing 3,5-disubstituted-2,4,6-triiodo aromatic amine represented by a formula (II), wherein R1 and R2 are defined in the instruction, and the compound represented by the formula (II) is a key intermediate for synthesizing iopamidol, iohexol, iodixanol and a series of non-ionic contrast agents. The method comprises: adopting a chlorine-free iodination reagent and a 3,5-disubstituted aromatic amine compound to carry out an iodination reaction to obtain the 3,5-disubstituted-2,4,6-triiodo aromatic amine represented by the formula (II), wherein a mole yield of the iodination reaction can be 89%.

The invention discloses a synthetic method for tildipirosin. The synthetic method comprises the steps that 20-piperidyl-5-O-mycaminose base-tylosin lactone silicon is subjected to alkylation protection and then has an iodination reaction with iodotrimethylsilane, and 20-piperidyl-23-I-5-O-mycaminose base-tylosin lactone is prepared and then synthesized with piperidine to obtain tildipirosin. The whole process route is simplified, reaction conditions are mild, the reaction is easy to control, the 23-digit allose base does not need long-time hydrolysis, the reaction time is shortened, the overall yield is increased and reaches up to more than 85%, and the product quality completely meets the related standard requirement.

The invention discloses a cholesterol molecular probe and a preparation method thereof. The cholesterol molecular probe shown as a formula (I) is prepared by taking lithocholic acid as a raw material through esterification reaction, oxidization reaction, dehydrogenation reaction, carbonyl protection reaction, reduction reaction, hydroxyl protection reaction, reduction reaction, iodination reaction, substitution reaction and de-protection reaction. The invention further discloses application of the cholesterol molecular probe shown as the formula (I) to identification of cholesterol modified protein. The cholesterol molecular probe provided by the invention can be used for simulating normal cholesterol to promote cell growth, and prompting the shearing ripening of the cholesterol modified protein hedgehog, and can also be used for researching cholesterol modification of the protein.

The invention discloses a method for preparing a Sacubitril intermediate of anti-heart-failure medicine as indicated in the formula (VII).The method comprises the following steps of taking D-phenylalanine which is low in price and easy to obtain as the raw material, and conducting an iodination reaction, an esterification reaction, a Boc protection reaction, a negishi coupling reaction, a DIBAL-H reduction reaction and a wittig reaction, so that the Sacubitril intermediate is obtained through preparation.The method for preparing the Sacubitril intermediate is mild in reaction condition and environmentally friendly, compared with existing preparation methods, the yield is higher, and the method is economical, effective and suitable for large-scale industrialized production.

The present invention provides a process for producing 5-iodo-2-methylbenzoic acid by iodizing 2-methylbenzoic acid, which comprises, as essential steps, a reaction step in which 2-methylbenzoic acid is iodized in the presence of a microporous compound, iodine, an oxidizing agent, and acetic anhydride and a purification step in which sublimation, distillation, crystallization, or a combination of two or more of these is conducted. By the process, 5-iodo-2-methylbenzoic acid, which is useful in functional chemicals such as medicines, can be easily obtained as a high-purity compound in a high yield. The production steps comprising reaction and separation/purification are simple from the standpoint of process operation and the purification load is small. Furthermore, the microporous compound, e.g., a zeolite catalyst, separated and recovered from the liquid resulting from the reaction can be repeatedly used after a simple treatment. Consequently, the catalyst has a long life and the target compound can be produced by the efficient process.

The invention relates to a method for preparing ceftazidime by a one-pot process. The method comprises the following steps: by using 7-aminocephalosporanic acid as the raw material, carrying out silanization reaction and iodination reaction, reacting with pyridine, directly adding the liquid into ceftazidime side chain acyl chloride hydrochloride to perform acylation reaction without separation to obtain ceftazidime iodate, adding the liquid into a concentrated hydrochloric acid-water mixed solution to perform deprotection, extracting to stratify, and regulating the pH value of the water phase with an alkaline solution to obtain ceftazidime (6R,7R)-7-[[(2-amino-4-thiazolyl)-[(1-carboxy-1-methylethoxy)imino]acetyl]amino]-2-carboxy-8-oxo-5-thia-1-azabicyclo[4,2,0]octyl-2-ene-3-methylpyridine pentahydrate. The method has the advantages of high yield, low cost, mild technological conditions, controllable technical process, high safety and low energy consumption, and is simple to operate.

The invention relates to a preparation method of an iodated chitosan oligosaccharide seaweed bio-fertilizer. The preparation method comprises the following steps of: (1) carrying out enzymatic hydrolysis reaction on chitosan, namely, shearing and crushing chitosan, and carrying out enzymatic hydrolysis reaction by using non-special composite enzyme so as to obtain a chitosan oligosaccharide solution with a molecular polymerization degree of 4-8; (2) carrying out iodination reaction on the chitosan oligosaccharide, namely, adding a potassium iodide solution into the obtained chitosan oligosaccharide solution in a certain speed, so as to carry out the iodination reaction on the chitosan oligosaccharide and obtain an iodated chitosan oligosaccharide solution; and (3) carrying out chelation reaction on a seaweed extract, namely, taking the seaweed extract which is prepared by using an enzymatic hydrolysis method, carrying out chelation reaction on the seaweed extract and the iodated chitosan oligosaccharide solution according to a certain ratio, and compounding microelements of certain concentration, and finally obtaining the iodated chitosan oligosaccharide seaweed bio-fertilizer. The iodated chitosan oligosaccharide seaweed bio-fertilizer prepared by using the method has the remarkable functions of plant growth promoting, production increase, disease-resistance and health care, also has the strong and lasting sterilization function, is free of residue and pollution, and is a completely environmental-friendly bio-fertilizer that the medicine and the fertilizer are combined together.

The invention discloses a preparation method of heptadecafluorooctyl iodoalkane, and belongs to the technical field of chemical synthesis. The preparation method comprises the following steps of: implementing a sulfonylation reaction on heptadecafluorooctyl potassium sulphonate at reacting temperature, to obtain heptadecafluorooctyl sulfonyl chloride after the reaction; implementing a bromination reaction on the heptadecafluorooctyl sulfonyl chloride at reacting temperature, to obtain heptadecafluorooctyl bromoalkane after the reaction; and implementing an iodination reaction on the heptadecafluorooctyl bromoalkane, to obtain heptadecafluorooctyl iodoalkane after the reaction. In comparison with the prior art, the preparation method of the heptadecafluorooctyl iodoalkane has the advantages of being simple in synthesis route, easily available in raw materials, moderate in processing conditions, lower in cost, and convenient for industrial production.

The invention discloses a BODIPY-containing bactericidal material and a preparation method and application thereof. The preparation method comprises that BODIPY-Br and sodium azide undergo a reactionto produce BODIPY-N3, BODIPY-N3 and acetylated maltoheptaose undergo a reaction under the catalytic action of a CuCl/PMDETA complex to produce BODIPY-Mal, and the BODIPY-Mal, iodic acid and iodine undergo an iodination reaction to produce the BODIPY-Mal-I bactericidal material. The BODIPY-Mal-I bactericidal material has good water solubility and completely retains the properties of BODIPY. The photodynamic power generated by BODIPY-Mal-I can effectively inactivate yeast cells and especially kill gram-positive bacteria. The preparation method has the advantages of simple processes, mild reaction conditions, low risk and low toxicity.

The invention relates to preparation methods of cefpirome intermediate and cefpirome; 7-amino cephalsporanic acid is used as a raw material; a silanization reaction, an iodination reaction, and a pyridine reaction are performed; the obtained product is added with an oxidant, and hydrochloric acid or is added into a mixed solvent of an organic solvent and water to prepare a halogen acid salt of the cefpirome intermediate (6R, 7R)-7-amino-3-[(2,3-cyclopentene-pyridine)methyl]ceph-3-ene-4-carboxylic acid. The invention also provides a method for preparing cefpirome sulfates by using the obtainedintermediate halogen acid salt. The cefpirome intermediate and cefpirome prepared by the methods have high yield, and low production cost; the operation is simple; the discharge of three wastes is less; treatment and recovery are easy, and the methods are applicable to industrial production.

Provided is a production method for an iodine compound in which iodine is reacted with a substrate in the presence of a porous material having a pore diameter of 500 nm or less or in the presence of the above porous material and an oxidizing agent and a production process for high purity 5-iodo-2-methylbenzoic acid comprising an iodination reaction step carried out by the above-mentioned, a crystal precipitation and separation step in which a product is precipitated by adding water or cooling and then separated and a purification step in which crystal separated is recrystallized using an organic solvent. According to the production method for an iodine compound described above, iodine can be introduced into various substrates at a high selectivity. Since expensive metals and specific reagents do not have to be used, it can readily be carried out in an industrially scale, and the product having a high purity can be obtained. Further, the process comprising the iodination reaction, separation and purification steps described above makes it possible to readily obtain at a high yield, 5-iodo-2-methylbenzoic acid having a high purity which is useful in uses for functional chemical products such as medicines. The process of the present invention comprising iodination reaction, separation and purification steps is characterized by that it is simple in terms of a procedure and that the purification load is smaller, and it is very advantageous in industrially carrying out.

The invention relates to a hafnium-base mixed metal material and an iodination preparation method thereof, and belongs to the field of synthesis and preparation of mixed metal materials. The hafnium-base mixed metal material is composed of a matrix metal hafnium and other metal compositions, and the other metal compositions comprise one or two or more of Zr, Ti, Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Ho, La, Mg, Mn, Mo, Nb, Ni, Pr, Sc, Sm, Sr, Ta, V, W, Y and Yb. The hafnium-base mixed metal material with the purity up to 99.95 wt% can be prepared through an iodination reaction, and continuous batch production can be realized, and the advantages of uniform product compositions, high production efficiency, relatively low production cost and the like are provided.

The application of the invention relates to preparation methods of iopromide and an intermediate of the iopromide. The method specifically comprises the following steps: conducting a reduction reaction, an iodination reaction and an acylation reaction on a compound shown in the formula VI to prepare a compound shown in the formula III, and further preparing to obtain the iopromide. The method notonly avoids the generation of double acylation byproducts, but also effectively reduces the generation of byproducts in the preparation process, the intermediate is easy to separate and purify, and ahigh-purity product is obtained at a relatively high yield.

The invention discloses a method for preparing a loxilan intermediate. 5-nitro-N-(2-hydroxyethyl)-m-formamide benzoic acid serving as an initial raw material is subjected to methyl esterification reaction with methanol, amidation reaction with 3-amino-1,2-propylene glycol in methanol solution, iodination reaction with iodine monochlorde in aqueous solution after the product of amidation reaction is reduced with ferric acid, acetylation reaction with acetic anhydride and hydrolysis in aqueous ammonia to obtain 5-acetamido-N-(2,3-dihydroxypropyl)-N-(2-hydroxyethyl)-2,4,6-triiodo-1,3-phthalic amide. The target compound can be obtained by acylation and hydrolysis reaction after the iodination reaction; the use of the expensive iodine monochlorde is avoided at the initial stage of the reactionsteps, so the cost of the whole reaction is greatly reduced; and the reaction condition is mild and the purity of the product is high because the aqueous ammonia is used in the hydrolysis reaction.

The invention relates to a preparation method of cefalonium. According to the preparation method, raw materials (cefalotin and pyrazinamide) react at a low temperature to obtain the product cefalonium. The preparation method particularly comprises the following steps: dissolving cefalotin acid into an organic acid, carrying out carboxyl protection by using a silanization protection reagent and then carrying out iodination reaction on reaction products and iodotrimethylsilane; then carrying out amination reaction on the reaction product from the former step and pyrazinamide; and finally carrying out deprotection by alcoholysis, regulating the pH value at a low temperature and crystalizing to obtain cefalonium. According to the preparation method of cefalonium, cefalotin acid is protected by the silanization protection reagent in an organic solvent and then reacts with iodotrimethylsilane; the reaction time is short, the reaction conditions are mild, the reaction is complete and no side reaction is almost generated; due to adoption of a mixed solvent crystallization method, the characteristics of high drying speed, light color and high yield can be achieved; in addition, the used solvent can be recycled and the amount of generated sewage can be reduced; therefore, the preparation method of cefalonium has remarkable economic and environmental benefits and facilitates industrial production.

The invention provides a preparation method of 1-fluoro-2-bromo-iodobenzene. The method comprises the steps that 1-fluorine-2-amidogen-3-nitrobenzene is used as a raw material, 1-fluorine-2-bromine-3-nitrobenzene is obtained through a diazotization and bromination reaction, 1-fluoro-2-bromo-aminobenzene is obtained through a following reduction reaction, and then 1-fluoro-2-bromo-iodobenzene is obtained through a diazotization and iodination reaction. According to the preparation method, under the acidic condition, 1-fluoro-2-bromo-aminobenzene and sodium nitrite react in a solvent, hydrogen iodide or iodate is added to the mixed solution, and 1-fluoro-2-bromo-iodobenzene is obtained through a reaction. The preparation method of 1-fluoro-2-bromo-iodobenzene is high in safety, mild in reaction condition, low in cost, easy to operate and industrialize and high in utilization rate of iodine.

The invention discloses a preparation method of 3-iodo-5-bromo-4, 7-diazaindole. The preparation method comprises the following steps that 1), 2-aminopyrazine and N-bromosuccinimide undergo a bromination reaction to produce 2-amino-3, 5-dibromopyrazine; 2) 2-amino-3, 5-dibromopyrazine undergoes a synthesis reaction in the presence of acetaldehyde, potassium tert-butoxide and an N-heterocyclic carbine-Pd (NHC-Pd) compound as a catalyst to produce 5-bromo-4, 7-diazaindole; and 5-bromo-4, 7-diazaindole undergoes an iodination reaction to produce 3-iodo-5-bromo-4, 7-diazaindole. The preparation method has the advantages that raw material prices are low; a reaction process route is short; a reaction yield is high; and products can be separated easily.

The invention relates to a preparation method of a quaternary ammonium salt type cationic povidone-iodine antibacterial material. The method comprises the following steps: (1) uniformly mixing vinyl pyrrolidone, a quaternary ammonium salt type cationic monomer, a hydrophobic comonomer and a silane coupling agent, adding an initiator, and carrying out ultrasonic mixing uniformly to obtain a mixed solution; (2) slowly dropwise adding the mixed solution into deionized water while stirring at a constant speed, and continuously reacting for 2-6 h at the temperature of 60-90 DEG C after drop-by-dropadding is finished so as to obtain a product A; (3) sequentially carrying out centrifugal separation, washing and freeze drying on the product A to obtain a quaternary ammonium salt type cationic polymer; and (4) under the protection of nitrogen, adding the quaternary ammonium salt type cationic polymer into an alcoholic solution of I2 for an iodination reaction to obtain a product B, performingwashing and suction filtration on the product B, and carrying out vacuum drying to obtain the product. The synthesis process is simple and efficient, and the obtained antibacterial material has broad-spectrum antibacterial activity and good biocompatibility and can be used for antibacterial research of products such as coatings, printing ink and dyes.

The present invention relates to a preparation method and intermediates of iopromide. The method specifically comprises: adopting a compound represented by a formula II as a starting raw material, and sequentially carrying out an acylation reaction, a lactonization reaction, a further acylation reaction, a reduction reaction, an iodination reaction, a re-acylation reaction and a final hydrolysis reaction to obtain the iopromide represented by a formula I, wherein a compound represented by a formula VII and a compound represented by a formula V are introduced as the intermediates so as to avoid the generation of the bismer by-product, the lactone ring is not easily subjected to ring opening removing during the iodination reaction process, and the introduced intermediates are easy to separate and purify, such that the high-purity iopromide can be prepared in the high-yield manner.

The invention provides acetylthiocholine iodide and a preparation method thereof. The preparation method comprises the following steps: step S1, dissolving a dimethylamino ethane compound in alkali toobtain an alkaline aqueous solution; step S2, adding a thioacetic acid compound into the alkaline aqueous solution to subject the thioacetic acid compound and the dimethylamino ethane compound to a thioreaction to generate (2-(dimethylamino)ethyl)ethanethioate; S3, separating the (2-(dimethylamino)ethyl)ethanethioate, and preparing an organic solution of the (2-(dimethylamino)ethyl)ethanethioate;and S4, dropwise adding an organic iodide into the organic solution of the (2-(dimethylamino)ethyl)ethanethioate for an iodination reaction so as to generate the acetylthiocholine iodide. According to the preparation method provided by the embodiment of the invention, the high-purity acetylthiocholine iodide can be obtained, and the titration content, the melting point, the clarity and other dataof the product are very excellent. The method is simple in operation, good in safety, suitable for industrial production, easy in raw material obtaining and low in cost.

The invention discloses a novel synthesis method of aromatic 5-chloro-2-fluoro-4-(trifluoromethyl) aniline hydrochloride containing a trifluoromethyl intermediate. The method comprises steps as follows: 1) 5-chloro-2-fluoroaniline, elemental iodine and the like are subjected to an iodination reaction in an anhydrous ethanol solution; 2) with dichloromethane as a solvent, an obtained aromatic iodination product is subjected to an acetylation reaction; 3) the aromatic iodination product protected by acetyl, methyl fluorosulphonyldifluoroacetate and the like are subjected to a trifluoromethylation reaction at the temperature of 80 DEG C; 4) finally, 6 mol/L hydrochloric acid is used for a deacetylation reaction in ethanol, and a target product is obtained. The novel synthesis method has the advantages that the route design is novel, the product purity is good and operation is safe, simple and convenient; all reactions are stably conducted in the solvent, the process is easy to control, few crude product impurities exist, purification is easy, and the quality and yield of the product are increased. The total yield of the route is 66%, the product purity can reach 98.5%, and the novel synthesis method has higher research and development application value.

The invention discloses a novel synthesis method for 2,5-dibromo-iodobenzene and belongs to the field of organic chemistry synthesis.The synthesis method includes the steps that with 1,4-dibromo-benzene being a starting raw material, trifluoroacetic acid and iodine are subjected to an iodination reaction to synthesize the target product 2,5-dibromo-iodobenzene.The method avoids low-temperature reaction, is easy to implement, generates a small number of by-products, is suitable for industrialized production and has good application prospects.2,5- dibromo-iodobenzene is an important fine chemical intermediate and is widely applied to the fields of synthesis medicine, pesticide, dye, plastics, functional polymer materials and others.