397 results about "Carbonyldiimidazole" patented technology

The invention relates to polyurethaneurea hydrogel and preparation methods therefor. The preparation methods comprise two preparation methods. The first preparation methods is as follows: diisocyanate and catalysts are added in a polyethylene glycol (PEG) organic solution for reaction, then diamine chain extender is added, and products are obtained in the organic solvent after precipitation, wherein, the molar ratio of PEG, diisocyanate and diamine is 1:2:1. The second preparation method is as follows: N,N'-dicarbonyl diimidazole is added in a PEG organic solution for reaction, then excess diamine chain extender is added, macromolecules with amidogens at two ends are obtained, finally, diisocyanate is added, and products are obtained in the organic solvent after precipitation, wherein, the molar ratio of PEG and diisocyanate is 1:2. The polyurethaneurea hydrogel has advantages of large elongation and high tensile strength, and has shape memory functions. The polyurethaneurea hydrogel has application prospects at aspects of biomedical hydrogel, tissue engineering, hydrogel support materials, biomedical devices with shape memory functions and the like.

The present invention relates to a novel process for the preparation of 3-hydroxy-N,1,6-trialkyl-4-oxo-1,4-dihydropyridine-2-carboxamide of formula I:The method comprises of the TEMPO oxidation of a primary alcohol of 3-O-protected-2-hydroxymethyl-6-alkyl-4H-pyran-4-one of formula III to 3-O-protected-6-alkyl-4-oxo-4H-pyran-2-carboxylic acid of formula II. Reaction of compound of formula II with methylamine and 1,1-carbonyldiimidazole in an inert solvent affords 3-O-protected-N,1,6-trialkyl-4-oxo-1,4-dihydropyridine-2-carboxamide, which is deprotected to give of 3-hydroxy-N,1,6-trialkyl-4-oxo-1,4-dihydropyridine-2-carboxamide of formula I.

An efficient synthesis for the preparation of N-[(3R,6S)-6-(2,3-difluorophenyl)-2-oxo-1-(2,2,2-trifluoroethyl)azepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide, by coupling (3R,6S)-3-amino-6-(2,3-difluorophenyl)-1-(2,2,2-trifluoroethyl)azepan-2-one and 2-oxo-1-(4-piperidinyl)-2,3-dihydro-1H-imidazo[4,5-b]pyridine dihydrochloride with 1,1′-carbonyldiimidazole (“CDI”) as carbonyl source; an efficient preparation of the potassium salt of N-[(3R,6S)-6-(2,3-difluorophenyl)-2-oxo-1-(2,2,2-trifluoroethyl)azepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide; efficient syntheses for the preparation of intermediates (3R,6S)-3-amino-6-(2,3-difluorophenyl)-1-(2,2,2-trifluoroethyl)azepan-2-one and 2-oxo-1-(4-piperidinyl)-2,3-dihydro-1H-imidazo[4,5-b]pyridine dihydrochloride, and the potassium salt of N-[(3R,6S)-6-(2,3-difluorophenyl)-2-oxo-1-(2,2,2-trifluoroethyl)azepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide including the potassium salt ethanolate and potassium salt hydrate.

The invention discloses a preparation method of a proton exchange membrane used for a direct methanol fuel cell. The method is realized by that polyether ether ketone is added into concentrated sulfuric acid to carry out sulfonation reaction, thereby obtaining sulfonated polyether ether ketone, then the sulfonated polyether ether ketone is dissolved in organic solvent, N, N (1)-Carbonyldiimidazole is added to stir for one to three hours, coupling agent is mixed for stirring the reaction for 1.5 to 4 hours, then inorganic crosslinking agent is mixed to react under the temperature of 50 to 80 DEG C. Proton conductors are mixed to continue getting the mixed solution of the sulfonated polyether ether ketone or the inorganic crosslinking agent or proton conductors under the temperature. Finally the proton exchange membrane for a direct methanol fuel cell is obtained by that the mixed solution of the sulfonated polyether ether ketone or the inorganic crosslinking agent or proton conductors is/are processed through membrane forming, drying and exuviation. The membrane has the advantages of good methanol diffusion resistance, low cost, high proton conductivity and good water-resistant swelling performance under high temperature. The preparation method is simple, the raw materials have low price, and the production cost is low.

The invention discloses a preparation method of pimavanserin. The method comprises the following two steps: firstly, 4-isobutoxy benzene methylamine and carbonyl diimidazole are subjected to acylation reaction to obtain N-(4-isobutoxy phenyl)-1H-imidazole-1-formamide, and the N-(4-isobutoxy phenyl)-1H-imidazole-1-formamide and N-(4-fluorophenyl)-1-methylpiperidine-4-amine are subjected to urea reaction, so as to obtain the pimavanserin. The prepared pimavanserin is good in quality and high in yield, the reagent toxicity is relatively low, the operation is simple and easy to control, and the pimavanserin is suitable for industrial production.

The invention discloses a method for modifying a nano metal oxide by coupling graft, and belongs to the technical field of nano granule surface modification. The nano metal oxide is used as a raw material, N,N'-carbonyl diimidazole (CDI) is used as an activating agent, and a finished product is obtained by simple processes of drying treatment, coupling reaction, separation and purification, coupling graft, re-separation and re-purification. The method has the advantages of simplicity, mild reaction conditions, high grafting efficiency which reaches 87 percent, energy conservation, emission reduction, low cost and suitability for large-scale industrial production. The nano metal oxide prepared by using the method can be widely applied in the fields of rubber, coating, ink, dye, glass, piezoelectric ceramics, photoelectrons, medicament and the like.

The invention relates to an endotoxin adsorbent, which in detail relates to a method of preparing endotoxin adsorbent for blood perfusion. The method employs spherical agarose gel with good biocompatibility as base material, employs epichlorohydrin, hexamethylene diamine, 1, 1'-carbonyldiimidazole as activating agent, and bonds polymyxin B for endotoxin removal. The invention is characterized in that it overcomes the toxicity of cyanogen bromide and instability of aglycone, improves the safty and reliability of operation, reducesnon-specific adsorption through bonding polymyxin B with 1, 1'-carbonyldiimidazole, and improves biocompatibility of adsorbent and suits for treating endotoxemia. The invention is also characterized by simple experimental procedure and high clearance for endotoxin.

The invention discloses a preparation method of double-targeting cationic ultrasound microbubbles carrying cell-penetrating peptide iRGD and belongs to the field of fundamental research. The preparation method uses materials, including DSPC, DSPE-PEG2000-maleimide, DSPE-PEG2000-Biotin, iRGD peptide, CCR2 antibody, stearic acid, branched-chain polyetherimide-600, N, N'-carbonyldiimidazole, and avidin; by bonding integrin Alpha v Beta3 targeting cell-penetrating peptide iRGD and the CCR2 antibody to surfaces of the microbubbles, double-targeting cationic ultrasonic contrast agent is constructed and has the double functions of carrying plasmid DNA and targeting tumor cells; combining ultrasound-mediated biological effect and iRGD cell-penetrating action, the agent is capable of promoting entry of genes into the tumor cells and improving gene transfection efficiency and is expected to be developed and applied to visual ultrasound-controlled-release genetic treatment of tumors.

The present invention provides a method for preparing a relugolix intermediate compound 8. The method comprises: (a) carrying out a reaction on a compound 2 and N,N'-carbonyldiimidazole to obtain a compound 3; (b) carrying out a reaction on the compound 3 and 2,6-difluorobenzyl chloride to obtain a compound 4; (c) carrying out a reaction on the compound 4 and 3-amino-6-methoxypyridazine to obtaina compound 5; (d) carrying out a reaction on the compound 5 and N,N'-carbonyldiimidazole to obtain a compound 6; (e) carrying out a reaction on the compound 6, N-bromosuccinimide and azobisisobutyronitrile to obtain a compound 7; and (f) carrying out a reaction on the compound 7 and dimethylamine hydrochloride to obtain a compound 8. The invention further provides a relugolix preparation method, which comprises: (g) carrying out a reaction on the compound 8 obtained by the method and hydrogen under a catalyst to obtain a compound 9; and (h) carrying out a reaction on the compound 9, N,N'-carbonyldiimidazole and methoxy amine hydrochloride to obtain relugolix. According to the present invention, the method adopts the route sequentially comprising loop closing and coupling, such that the method has characteristics of simple operation, less side-reaction, mild reaction condition, high yield, high product purity and easy product purification, and is suitable for commercial scale production.

The invention discloses a preparation method of an azilsartan intermediate shown as in the formula I. According to the invention, the intermediate shown as in the formula I is obtained through a condensation cyclization reaction between a compound shown in the formula II and N, N'-carbonyl diimidazole or bis (trichloromethyl) carbonate in an aprotic solvent. Organic alkali can be added in the above reaction system to improve the reaction rate. The preparation method of the azilsartan intermediate shown as in the formula I has the advantages of high yield and low cost.

The invention discloses a preparation method of a pharmaceutical intermediate, i.e., sodium 8-[(2-hydroxybenzoyl) amino] octanoate. The preparation method comprises the steps of enabling salicylamide,used as a raw material, to react with N' N-carbonyl diimidazole so as to generate an intermediate, i.e., 2H-benzo[e][1,3]oxazine-2, 4 (3H)-dione; enabling the intermediate to react with 8-ethyl bromooctanoate to obtain 8-(2, 4-dicarbonyl-2H-benzo[e][1, 3]oxazine-3(4H)-yl) ethyl caprylate; hydrolyzing by using sodium hydroxide, and then acidizing to obtain 8-[(2-hydroxybenzoyl) amino] caprylic acid; then, enabling the 8-[(2-hydroxybenzoyl) amino] caprylic acid to react with sodium hydroxide to obtain the final product, i.e., the sodium 8-[(2-hydroxybenzoyl) amino] octanoate. The preparation method avoids the use of a genotoxic raw material-ethyl chloroformate, is low in reaction energy consumption, less in by-products and high in yield, greatly lowers the production cost, and is simple inprocess and suitable for industrial production.

The invention discloses a method for preparing quinolone medicaments. The conventional methods using organic solvents with a high boiling pint and a large polarity, adopting other solid alkali materials except reaction materials or using other liquid alkali materials except the reaction materials have obvious defects. The method of the invention adopts a technical scheme that: quinolone compounds are prepared by a piperazidine reduction of quinolone carboxylate nuclear parent and piperazidine derivates in water; the piperazidine reduction is completed in the presence of a catalyst which may be one or a mixture of more than two of cerous chloride heptahydrate, N,N-carbonyldiimidazole, 4-dimethylamino pyridine, tetrabutylammonium bromide, benzyl triethylammonium chloride and tetrabutyl ammonium hydroxide. The method for preparing the quinolone medicaments radically solves the problems of terrible smell, realizes clean production, avoids using the other alkali substances except the reaction materials as an acid-binding agent and overcomes the defects of the prior art.

The invention relates to a staphylococcal protein A (SPA) immunoadsorption material used for blood purification and a preparation method thereof. The invention discloses a macromolecule material which is coupled by agarose gel and SPA. The material is prepared by taking the agarose gel as carrier substrate which is reacted with epoxy bromopropane to obtain the epoxy-based active carrier; after that, polyamines reagent is taken as a space arm which is then reacted with carbonyl diimidazole and is then coupled with the SPA. The material has the advantages of short synthesis time, safe preparation, strong specificity of product, high adsorption efficiency and good regeneration performance to immunoglobulin and the compound thereof, and being able to be applied to clinic immunoadsorption cure.

The invention discloses a synthetic method for avibactam sodium salt. The method comprises the following steps: taking (2S, 5R)-5-[(benzyl oxyl) amino] piperidine-2-formamide as a starting material; constructing a urea ring by carbonyl diimidazole under the effect of dimethyldichlorosilance to obtain (2S, 5R)-6-(benzyl oxyl)-7-oxo-1,6-diazabicyclo [3.2.1] octane-2-formamide; then carrying out hydrogenation to remove benzyl; carrying out sulfonation reaction on the compound and a sulfonated reagent; synthesizing into a quaternary ammonium salt intermediate by using quaternary ammonium salt; and finally carrying out ion exchange to obtain the avibactam sodium salt. The improved process is low in cost, simple and convenient to operate, good in product quality and suitable for industrial production. In a process of synthesizing the intermediate (2S, 5R)-6-(benzyl oxyl)-7-oxo-1,6-diazabicyclo [3.2.1] octane-2-formamide, dimethyldichlorosilance which is low in price is used, and therefore, the production cost is greatly reduced.

The invention belongs to the field of polymer functional membrane materials, and particularly relates to an ion exchange membrane for a proton exchange membrane fuel cell (PEMFC) and a vanadium redox battery (VRB), in particular to a cross-linking perfluorinated sulfonic acid ion exchange membrane and a preparation method thereof. The method comprises the following steps: dissolving carbonyldiimidazole and perfluorinated sulfonic acid ion exchange resin into an organic solvent to prepare perfluorinated sulfonic acid solution (perfluorinated membrane casting solution); adding a cross-linking agent into the membrane casting solution, mixing well, and pouring the membrane casting solution onto the surface of a horizontal glass plate or a Hastelloy alloy steel plate, thereby preparing a cross-linking ion exchange membrane. The cross-linking perfluorinated sulfonic acid ion exchange membrane prepared in the invention has oxidation resistance, good dynamic stability and good mechanical stability, and can effectively reduce the cost of the battery and promote the commercial popularization of the battery.

The invention discloses a method for preparing high-purity torasemide and a crystal form I thereof. The method comprises the following steps of: reacting 4-chloro-3-pyridine sulfonamide and m-toluidine serving as raw materials to obtain 3-sulfamoyl-4-(3-methyl phenyl) aminopyridine, refining, and reacting with 1,1'-carbonyldimidazole and isopropamide, directly introducing isopropyl carbamyl, thus obtaining the high-purity torasemide, wherein the purity (high performance liquid chromatography (HPLC)) of the torasemide is more than 99.5 percent. The prepared torasemide has proper granularity, seed crystal is not required for crystal transformation, the torasemide can be directly transformed into the variant crystal form I, and a chemically pure torasemide variant I is obtained. The preparation method is strong in process controllability, easy and convenient to operate and high in reproducibility, and facilitates industrialized production.

The invention relates to a hydrogel which is temperature-sensitive and biodegradable simultaneously, the hydrogel is prepared by the following method: hydroxyethyl methacrylate-polycaprolactone is obtained by the reaction of hydroxyethyl methacrylate and epsilon-caprolactone; the hydroxyethyl methacrylate-polycaprolactone reacts with carbonyldiimidazole, hydroxyethyl methacrylate-polycaprolactone-imidazole is obtained by rotary evaporation; the hydroxyethyl methacrylate-polycaprolactone-imidazole and Alpha-(1->6)-D-glucan are dissolved in dimethyl sulfoxide, p-dimethylaminopyridine is added, mixture which is obtained by the reaction at room temperature is settled in isopropyl alcohol, hydroxyethyl methacrylate-polycaprolactone-g-Alpha-(1->6)-D-glucan is obtained by vacuum drying; N-isopropylacrylamide and the hydroxyethyl methacrylate-polycaprolactone-g-Alpha-(1->6)-D-glucan are dissolved in phosphorous acid buffer solution with pH of 7.4, then ammonium persulfate and N,N,N',N'-tetramethylethylenediamine are added, the hydrogel is obtained by the reaction at room temperature; dialysis is carried out on the obtained hydrogel by phosphorous acid buffer solution, thereby obtaining the temperature-sensitive and biodegradable hydrogel.

The invention relates to a construction method of medical titanium alloy implant surface antibiotics slow release system. At first, titanium beads or titanium is mixed with an additive, and then the mixture is coated on the surface of prosthesis and titanium beads are sintered together by sintering, and at the same time, the titanium beads are sintered with the prosthesis; after being washed by ultrasound, the matter is immerged into the hydrogen peroxide solution, and then after being washed by the acetone solution, the matter is put into the carbonyldiimidazole acetone solution, and then after being washed by acetone solution, the matter is put into the sodium bicarbonate solution with dissolved RGD, then is washed by PBS after being taken out. Drugs curing and preventing bone infection and gelatin are combined into drug-loaded microspheres, then the drug-loaded microspheres are combined with the micro-porous layer on the surface of the prosthesis by protein cross-linker, thus obtaining the medical titanium alloy implant surface antibiotics slow release system. The medical titanium alloy implant surface antibiotics slow release system of the invention improves the physical absorption on metal surface and the chemical bond binding capacity, and stable combination strength between the low release microspheres and the implant can be obtained along with the function of the protein cross-linker.