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45 results about "Benzyl-EDTA" patented technology
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Polishing composition
InactiveCN101496143AFull grinding speedImprove flatnessOther chemical processesSemiconductor/solid-state device manufacturingEthylenediamineEthyl group
Disclosed is a polishing composition which realizes both high planarity and reduction of corrosion in the surface of a wiring metal. Specifically disclosed is a polishing composition containing an oxidizing agent (A), at least one or more acids (B) selected from amino acids, carboxylic acids having 8 or less carbon atoms and inorganic acids, a sulfonic acid (C) having a concentration of not less than 0.01% by mass and an alkyl group having 8 or more carbon atoms, a fatty acid (D) having a concentration of not less than 0.001% by mass and an alkyl group having 8 or more carbon atoms, and at least one or more compounds (E) selected from pyridinecarbonyl compounds, nonionic water-soluble polymers, 2-pyrrolidone, N-methylpyrrolidone, 1,3-dimethyl-2-imidazolidinone, gramine, adenine, N,N'-diisopropylethylenediamine, N,N'-bis(2-hydroxyethyl)ethylenediamine, N,N'-dibenzylethylenediamine and N,N'-diphenylethylenediamine.
Owner:SHOWA DENKO KK
Flucloxacillin sodium compound and preparation thereof
InactiveCN101475578AHigh purityImprove product qualityAntibacterial agentsOrganic chemistryPurification methodsFlucloxacillin sodium
The invention discloses a flucloxacillin sodium compound and a method for preparing the same. The method comprises that: firstly, N'N-dibenzylethylene diamine salt and flucloxacillin acid are mixed and reacted to form a salt; and secondly, high-purity flucloxacillin sodium is obtained through the displacement of a cation exchange resin. The invention adopts a purification method which is simple and easy to operate, thereby greatly improving the purity of the flucloxacillin sodium compound to a certain degree, removing a large amount of high molecular polymers, stabilizing the product quality of related preparations and ensuring the safety of clinic medication use.
Owner:海南本创医药科技有限公司
Synthetic method of N,N'-dibenzyl-1,2-ethanediamine
ActiveCN106748813AHigh selectivityAvoid PolymerizationOrganic compound preparationAmino compound preparationHydrogenation reactionBenzyl-EDTA
The invention discloses a synthetic method of N,N'-dibenzyl-1,2-ethanediamine. The synthetic method comprises the following components: in a reaction vessel, a liquid phase catalytic hydrogenation reaction is carried out for N,N'-dibenzylidene-1,2-ethanediamine in the effects of a nitrogen doped meso pore carbon loaded precious metal catalyst in order to prepare and obtain N,N'-dibenzyl-1,2-ethanediamine. In the nitrogen doped meso pore carbon loaded precious metal catalyst, the precious metal is Pd or Pt, and the load capacity of the precious metal is 1-10wt%. The synthetic method has the advantage of high selectivity of target products.
Owner:ZHEJIANG UNIV OF TECH
Palladium/active carbon catalyst and application thereof in synthesizing N,N'-dibenzylethylenediamine
ActiveCN102179245AIncrease profitOvercome the disadvantage of producing a large amount of waste acidOrganic compound preparationAmino compound preparationEthylenediamineBenzyl-EDTA
The invention discloses a palladium / active carbon catalyst and application thereof in synthesizing N,N'-dibenzylethylenediamine. The palladium / active carbon catalyst is prepared by the following steps of: impregnating active carbon by using aqueous solution of sodium halide, filtering, and washing a filter cake until halogen ions are absent; impregnating the treated active carbon by using aqueoussolution of H2PdCl4; and regulating the pH value of the solution until the solution is alkaline, filtering, washing a filter cake until the filter cake is neutral, and reducing the filter cake by using a reducing agent, and drying the obtained neutral product to obtain the palladium / active carbon catalyst. The palladium / active carbon catalyst has controllable size, most palladium particles in thecatalyst have the particle size of 2 to 5nm, the catalyst is used for synthesizing the N,N'-dibenzylethylenediamine by N,N'-dibenzylidene ethylenediamine through catalytic hydrogenation reduction, and has high activity, selectivity and stability; moreover, the catalyst is easy to prepare, environment-friendly and suitable for industrial application, and precious metal palladium is easy to recover.
Owner:嘉善县国创新能源研究院
Preparation method of cefoxitin
InactiveCN102633819AOvercoming the drawbacks of 101613361Avoid condensation side reactionsOrganic chemistrySodium methoxideHypochlorite
The invention relates to a preparation method of cefoxitin. The method comprises the following steps: adding a solvent A into a compound aqueous solution with the structure shown in the formula (IV), adding N,N'-dibenzylethylenediamine diacetate or aqueous solution thereof, filtering to obtain a compound with an intermediate structure shown in the formula (III); adding the compound with the intermediate structure shown in the formula (III) into acetone or tetrahydrofuran, adding chloriosulfonyl isocyanate to react, and hydrolyzing; adding acetic ether, filtering, extracting, decoloring, salting out, and filtering to obtain a compound with an intermediate structure shown in the formula (II); adding the compound with the intermediate structure shown in the formula (II) into an organic solvent B, adding organic acid to dissolve, adding a methanol solution with sodium methoxide and tert-butyl hypochlorite to perform methylation reaction, adding sodium pyrosulfite and acetic acid for neutralizing, adding water for extracting, acidifying water phase, filtering to obtain cefoxitin. According to the preparation method, deacetyled cefoxitin always exists in a mode of sodium salt or amine salt, so that the condensation side reaction easily caused by low pH can be avoided, and the product quality and yield can be well controlled.
Owner:山东安弘制药有限公司
Method used for high efficiency preparation of N,N'-dibenzylethylenediamine (DBE) through catalytic hydrogenation
ActiveCN108218718AReduced activityInhibition of hydrogenolysis reactionPhysical/chemical process catalystsOrganic compound preparationEthylenediamineSulfur
The invention discloses a method used for high efficiency preparation of N,N'-Bis(phenylmethyl)-1,2-ethanediamine (DBE) through catalytic hydrogenation. The method comprises a following step: in a reaction vessel, N,N'-dibenzylidene ethylenediamine is subjected to liquid phase catalytic hydrogenation under the catalytic effect of a nitrogen / sulfur codoped mesoporous carbon loaded noble metal catalyst so as to obtain DBE. The method is high in target product selectivity.
Owner:浙江辰阳化工有限公司
Preparation method of N,N-dibenzyl-ethylenediamin diacetate
InactiveCN101747206AGood technical effectSignificant technical effect: the method operation of the present inventionOrganic compound preparationAmino compound preparationEthylenediamineChemical synthesis
The invention relates to the field of chemical synthesis, in particular to a preparation method of N,N-dibenzyl-ethylenediamin diacetate. The preparation method comprises the following steps of: a: condensing reactants of benzaldehyde, ethylenediamine and glacial acetic acid into N,N-dibenzylidene ethylenediamine in an organic solvent; b: carrying out catalytic hydrogenation on the N,N-dibenzylidene ethylenediamine to obtain N,N-Dibenzylethylenediamine; and c: salifying the N,N-Dibenzylethylenediamine in the organic solvent to obtain the N,N-dibenzyl-ethylenediamin diacetate. The method has the advantages of simple and convenient operation, high product yield, low content of product impurity and no pollution to the environment, overcomes the defects existing in the prior art and has wide market prospect.
Owner:何永平
Cefuroxime dibenzyl ethylenediamine salt and preparation method and application thereof
ActiveCN101157697AImprove qualityAvoid Freezing RequirementsOrganic chemistryEthylenediamineCefuroxime
The invention provides a novel compound of cefuroxime dibenzyl ethylenediamine salt and a preparation method as well as the method for the preparation of cefuroxime dibenzyl ethylenediamine salt or purification of cefuroxime or cefuroxime salt.
Owner:SHANDONG SALUBRIS PHARMA +1
Synthesis of austrastaph
ActiveCN1613859ASimple processSimple and fast operationOrganic chemistryPenicillin synthesisOrganic solvent
Synthesis of cloxacillin benxethine is carried out by: dissolving 6-aminopenicillanic acid in aqueous organic solvent to form a sodium salt, condensing with o-chlorbenzylisoxazoleacyl cyanide to obtain cloxacillin benxethine solution directly, and having metathesis with N,N-dibenzyl quadol diacetate. It is simple and costs low.
Owner:石药集团中诺药业(石家庄)有限公司
Supported double-metal catalyst capable of efficiently synthesizing DBE (Dibasic Ester) and preparation method of supported double-metal catalyst
InactiveCN108970632AHigh selectivityAvoid PolymerizationPhysical/chemical process catalystsOrganic compound preparationActivated carbonAlkalinity
The invention discloses a supported double-metal catalyst capable of efficiently synthesizing DBE (Dibasic Ester) and a preparation method of the supported double-metal catalyst. The supported double-metal catalyst comprises a carrier, an active component and an auxiliary agent, and is characterized in that the carrier is nitrogen-doped activated carbon; the active component is noble metal; the auxiliary agent is Sn; the loading amount of the heavy metal is 1 to 10 weight percent and the loading amount of the Sn is 1 to 5 weight percent. According to the supported double-metal catalyst disclosed by the invention, a nitrogen element in the nitrogen-doped activated carbon carrier can provide suitable alkalinity to inhibit C-N hydrogenolysis reaction, polymerization reaction of N,N'-dibenzylideneethylenediamine and the like, so that the selectivity of a target product DBE is easy to improve.
Owner:浙江辰阳化工有限公司
Benzathine salt of ceftiofur, preparation method and application thereof
ActiveCN101245078AAvoid degradationReduce solubilityOrganic chemistryEthylenediamineCeftiofur sodium
The invention relates to the double benzyl (or the substituted benzyl) ethylenediamine salt of Ceftiofur, the preparation method and the application in the preparation of ceftiofur sodium salt. The double benzyl (or the substituted benzyl) ethylenediamine salt of Ceftiofur is adopted for the preparation of ceftiofur sodium by the treatment of cation resin, the preparation process and the processing are simple, the purity of products is high and the technique is stable, thus being suitable for the industrial production.
Owner:QILU ANIMAL HEALTH PROD +1
Preparation methods of dibenzyl ethylenediamine and acetate thereof
InactiveCN101774927AReduce stepsReduce wash extractionCarboxylic acid salt preparationAmino compound preparation by condensation/addition reactionsAcetic acidEthylenediamine
Owner:CHONGQING CITY CHUNRUI PHARMA CHEM
Method for preparing tardocillin
The invention discloses a preparing method of benzathine penicillin which comprises the following procedures: a, 50 percent to 75 percent of ethanol is added to a raw medicine of the N, N-dibenzyl ethylenediamine diacetate, and is prepared into solvent A; b, 50 percent to 75 percent of ethanol is added to the raw medicine of penicillin G salt, and is prepared into solvent B; c, the pre-applied solvent A is added to the solvent B for stirring, then the residual solvent A is added to the solvent B, thus obtaining nzathine benzylpenicillin suspension; d, filtering and then washing and drying are carried out on the nzathine benzylpenicillin suspension. The method has the advantages of improving yield coefficient of products, purity quotient and the controllability of particle size, reducing the toxicity of the residual solvent, improving the quality and safety of products and avoiding the harm of methanol to environment and human body at the same time.
Owner:NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
Method for preparing cefonicid dibenzylethylenediamine salt
InactiveCN102757450AShort reaction timeThe reaction process steps are simpleAmino preparation from aminesEthylenediamineChloride
The invention discloses a method for preparing a cefonicid dibenzylethylenediamine salt. The method comprises the following steps of: (1) adding an alkali into 7-ACA-3-SMT in water for dissolving, and reacting with D-(-)-formyl phenylacetyl chloride; (2) cooling a reaction liquid below 20 DEG C below zero, and adding an alkali for reacting; and (3) cooling the reaction liquid treated in the step (2), adding hydrochloric acid for adjusting the pH value, and reacting with N, N'-dibenzyl ethylenediamine diacetate to obtain a cefonicid dibenzylethylenediamine salt. The invention provides a method for preparing a cefonicid dibenzylethylenediamine salt, which has the advantages of low-temperature reaction, short reaction time, simple post-treatment and high product quality.
Owner:GUANGDONG LIGUO PHARMACY
Method for refining cefonicid dibenzyl ethylenediamine salts
ActiveCN109232610AHigh purityLess impuritiesOrganic compound preparationAmino compound preparationEthylenediamineIon exchange
The invention discloses a method for refining cefonicid dibenzyl ethylenediamine salts and belongs to the technical field of medicines. The method comprises the following steps: performing ion exchange on crude cefonicid salts with resins, decoloring the salts with a decoloring agent, carrying out a salt forming reaction with a transamination agent, and crystallizing by a precipitator, thereby obtaining the refined cefonicid dibenzyl ethylenediamine salts. The cefonicid dibenzyl ethylenediamine salt prepared by the method disclosed by the invention is high in purity, less in impurity and low in color grade, and the refining method disclosed by the invention has the advantages of being simple in process, energy-saving, environmental-friendly, suitable for large-scale industrial production and the like.
Owner:NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
Method for preparing cephapirin benzathine
The invention discloses a new method for preparing cephapirin benzathine by a one-pot method, relating to the field of chemical drug synthesis. The method comprises the following steps of: taking acetyl bromide 7-ACA as raw materials; in a solvent, in the presence of organic alkali, reacting the acetyl bromide 7-ACA with 4-pyridinethiols to obtain solid cefapirin acid; and then adding the organic alkali in the reaction liquid, dissolving the cefapirin acid as salt, and simultaneously and unnecessarily adding a reductant which is sodium thiosulfate, sodium hydrogensulfite or vitamin C; and then adding a reagent A in the reaction liquid, reacting the cefapirin acid salt with the reagent A at 0-50 DEG C for 0.1-20 hours to obtain the cephapirin benzathine, wherein the reagent A is dibezylethylenediamine diacetate acetate or dibezylethylenediamine diacetate. The method solves the problems that a product is easily decomposed, color is easily deepened in the process of preparing cefapirin sodium salt, and the like. The invention is simplified in steps, easy to operate and suitable for industrialized production, and the quality of the product accord with the quality standard of USP29.
Owner:GUANGZHOU BAIYUNSHAN PHARM CO LTD
HPLC measuring method for three ingredients of trinary mycin for injection
The invention relates to an HPLC measuring method for three ingredients of trinary mycin for injection. The HPLC measuring method comprises the following steps: 1), preparation of a reference solution; 2), preparation of a test solution; 3), chromatographic conditions, wherein the chromatographic column is a C18 reversed-phase chromatographic column, the mobile phase is a buffer salt solution-acetonitrile of which the volume ratio is 81:19, the buffer salt solution contains 0.21 mol / L of monopotassium phosphate and 0.16 percent of triethylamine, the pH value is 5.6, the flow velocity is 1.0 ml / min, the detection wavelength is 215 nm, and the sample size is 10 [mu]l; 4), content calculation, wherein the content calculation method adopts the external standard method, and the contents of procaine, dibenzyl ethylene diamine and penicillin in a test sample are calculated according to peak areas. According to the HPLC measuring method, the contents of the three ingredients of the trinary mycin can be measured at the same time, and the HPLC measuring method has the advantages of high repeatability, sensitivity and accuracy, and facilitates standard operation.
Owner:陈汝红
Medicinal composition containing ceftiofur bisbenzylethylenediamine
InactiveCN102885820ALow costImprove stabilityAntibacterial agentsOrganic active ingredientsBacterial respiratory infectionCeftiofur sodium
The invention provides a suspension injection of ceftiofur bisbenzylethylenediamine, which comprises the following components: 1.2% to 12.6% (w / v) of superfine powdery ceftiofur bisbenzylethylenediamine and 0.1% to 25% (w / v) of buffering agent, and the invention also provides the preparation steps of the suspension injection of ceftiofur bisbenzylethylenediamine. The invention discloses the suspension injection of ceftiofur bisbenzylethylenediamine and the medicinal value of the suspension injection of ceftiofur bisbenzylethylenediamine, namely at least the efficacy of ceftiofur is achieved. The suspension injection of ceftiofur bisbenzylethylenediamine provided by the invention can be prepared into the easily absorbed aqueous liquid dosage forms for treating bacterial respiratory infection of livestock, such as the preparation and oral liquid. Compared with the prior art, the suspension injection has the advantages that at least a step of preparing ceftiofur sodium by ceftiofur bisbenzylethylenediamine is saved, and the problems that the preparation steps of ceftiofur sodium are complicated and the cost is high are avoided.
Owner:LUOYANG HUIZHONG ANIMAL MEDICINE
Synthesis process of o-chloro-benzathine penicillin
InactiveCN105566349AOvercome serious pollution problemsIncrease conversion rate per passOrganic chemistryEthylenediamineDecomposition
The invention discloses a synthesis process of o-chloro-benzathine penicillin. 6-aminopenicillanic acid is firstly dissolved in a dilute alkali solution to be prepared into sodium salt in an aqueous solution of an organic solvent, then subjected to condensation with isoxazolyl o-chlorobenzoyl chloride to directly obtain a cloxacillin sodium solution, and the cloxacillin sodium solution is subjected to double decomposition reaction with N, N-dibenzyl ethylenediamine diacetate to obtain the o-chloro-benzathine penicillin. The synthesis process of the o-chloro-benzathine penicillin disclosed by the invention has benefits of simple process, simple and convenient operation, low cost and easy industrial production.
Owner:QINGDAO SHOUTAI AGRI SCI & TECH CO LTD
Method for preparing cefonicid dibenzyl ethylenediamine salt
The invention discloses a method for preparing cefonicid dibenzyl ethylenediamine salt. The method comprises the steps of A, acylation reaction, wherein 7-amino-3-(1-methylsulfonyl-1H-tetrazole-5-yl-s-methyl)-cephem-2-carboxylic acid is added to a pure water system, weak aqua ammonia is added for dissolution, a phase transfer catalyst is added, and D-(-)-formyl mandeloyl chloride and weak aqua ammonia are added dropwise to control pH for reaction so as to obtain a formyl cefonicid acid aqueous solution; B, deformylation, wherein the formyl cefonicid acid aqueous solution obtained in the step A is heated to 25-35 DEG C, acid liquor is added for hydrolysis reaction for 3-9 h, and a cefonicid acid aqueous solution is obtained after complete hydrolysis; C, salifying, wherein a N,N-dibenzyl ethylenediamine diacetic acid solution is added to the cefonicid acid aqueous solution obtained in the step B, and stirring crystallization is conducted to obtain the high-purity cefonicid dibenzyl ethylenediamine salt. By the adoption of the method, emission reduction is achieved from the source, environment friendliness is realized, operation is easy, production cost is reduced greatly, and economic benefits and social benefits are high.
Owner:NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
Sulfur carbon sphere-supported noble metal catalyst and its preparation and application in synthesis of N, N'-dibenzylethylenediamine
InactiveCN109012716AGood dispersionWell-developed microporous structurePhysical/chemical process catalystsOrganic compound preparationReaction rateSulfur
The invention discloses a sulfur carbon sphere-supported noble metal catalyst and its preparation and application in synthesis of N, N'-dibenzylethylenediamine. The catalyst is composed of sulfur carbon spheres and an active component supported on the surface of the sulfur carbon sphere. The S of the sulfur carbon sphere exists in the form of a C-S bond on the sulfur carbon sphere skeleton and surface. The mass ratio of S to C is 0.05 to 10%. The active component comprises platinum group metal particles with particle diameters of 4 to 10nm. Based on the sulfur carbon sphere mass, the loading ratio of the active component is 5-20%. The sulfur carbon sphere-supported noble metal catalyst is spherical, and has the particle diameter of 100-1000nm, a pore volume of 0.15-1.0ml / g, a specific surface area of 300-1000m<2> / g, an average pore diameter of 0.5-2nm and a micropore ratio of 60-85%. The sulfur carbon sphere-supported noble metal catalyst has the characteristics of high conversion rate, high catalytic activity, high stability and high reaction rate in preparation of N, N'-dibenzylethylenediamine shown in the formula (II) through catalytic hydrogenation reduction of N, N'-dibenzylidene ethanediamine.
Owner:ZHEJIANG UNIV OF TECH
Preparation method of chlorazol benzathine benzylpenicillin
ActiveCN102690277AReduce storageReduce embeddingOrganic compound preparationAmino compound preparationInjectable SuspensionBenzyl-EDTA
The invention relates to a preparation method of chlorazol benzathine benzylpenicillin, which comprises the following steps of: (a) measuring and taking the following materials of 1.0g of cloxacillin sodium, 2.0-10.0ml of water and 0.5-10.0ml of buffer agent according to the mass volume ratio to prepare solution A; (b) measuring and the taking the following materials of 1.0g of N, N'-DBED, 2.0-10.0ml of water and 1.0-10.0ml of buffer agent according to the mass volume ration to prepare solution B; (c) adding 15-30 percent of the total amount of the solution A into the solution B, reacting under a stirring state to generate crystal, and growing the crystal for 10-30 minutes; and flowing the rest solution A into the solution B within 30 minutes, and carrying out salt forming reaction to obtain chlorazol benzathine injectable suspension; and (d) filtering, washing, leaching, and vacuum drying at 50-80 DEG C to obtain the product. Stable degree of supersaturation is kept during the reaction, and the nucleus formation caused by outbreak of the product is effectively controlled, so that the product quality can be improved.
Owner:NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
Carboxylic acid penicillin amine salt and application thereof in preparing high-purification sodium oxacillin salt
The invention relates to a carboxylic acid penicillin dibenzyl (substituting benzyl) ethylenediamine salt compound and an application thereof in preparing a high-purification sodium oxacillin salt. The carboxylic acid penicillin dibenzyl (substituting benzyl) ethylenediamine salt compound has a structure as the formula II, and carboxylic acid penicillin comprises ticacillin, carbenicillin and thelike, wherein R is thiofuran-3-group or phenyl; R1, R2 and R3 are respectively independent H, alkyls of C1-C5, halogens and nitryl; and substituent groups of the substituted alkyl are selected from the halogens and alkoxy groups of C1-C5.
Owner:QILU PHARMA HAINAN +1
Green preparing method for high-purity N,N'-dibenzyl ethylenediamine diacetate
ActiveCN108752216AEmission reductionAchieve recyclingOrganic compound preparationCarboxylic acid salt preparationAcetic acidETHYLENEDIAMINE DIHYDROCHLORIDE
The invention relates to a green preparing method for high-purity N,N'-dibenzyl ethylenediamine diacetate. A by-product N,N'-dibenzyl ethylenediamine dihydrochloride or N,N'-dibenzyl ethylenediamine sulfate generated in the production process of long-acting cephalosporin medicine is used, and is neutralized, extracted and concentrated, then the product and acetic acid are mixed to form salt, and the high-purity N,N'-dibenzyl ethylenediamine diacetate is prepared. According to the green preparing method, discharging of liquid and solid waste is reduced, regeneration of the N,N'-dibenzyl ethylenediamine diacetate and recycling of waste are achieved, generation of the by-product or waste is reduced from the source, and therefore the aim of protecting and improving the environment is achieved.Compared with a traditional preparing method, the green preparing method has the advantages that the raw material is easy to obtain, the technology is simple, operation is easy and convenient, the production cost is low, and the green preparing method is more suitable for industrial production.
Owner:重庆天地药业有限责任公司
Method for efficiently synthesizing DBE through supported bimetallic catalyst
InactiveCN109046363ASmall metal particle sizeHigh catalytic activityOrganic compound preparationCatalyst activation/preparationHydrogenation reactionReaction speed
The invention discloses a method for efficiently synthesizing DBE through a supported bimetallic catalyst. The method comprises the following step: ensuring that N,N-dibenzylidene quadrol is subjectedto liquid phase catalysis hydrogenation reaction under the action of an active carbon supported bimetallic catalyst in a reaction kettle, so as to form the DBE. The method can further enhance the activity of the catalyst on the basis of guaranteeing the high selectivity of a target product, and has the advantages of high reaction speed and high selectivity of the target product.
Owner:浙江辰阳化工有限公司
Method for preparing tardocillin
The invention discloses a preparing method of benzathine penicillin which comprises the following procedures: a, 50 percent to 75 percent of ethanol is added to a raw medicine of the N, N-dibenzyl ethylenediamine diacetate, and is prepared into solvent A; b, 50 percent to 75 percent of ethanol is added to the raw medicine of penicillin G salt, and is prepared into solvent B; c, the pre-applied solvent A is added to the solvent B for stirring, then the residual solvent A is added to the solvent B, thus obtaining nzathine benzylpenicillin suspension; d, filtering and then washing and drying arecarried out on the nzathine benzylpenicillin suspension. The method has the advantages of improving yield coefficient of products, purity quotient and the controllability of particle size, reducing the toxicity of the residual solvent, improving the quality and safety of products and avoiding the harm of methanol to environment and human body at the same time.
Owner:NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
Pemetrexed-N,N-dibenzylethylenediamine salt and preparation method thereof
ActiveCN104817563AImprove stabilityThe manufacturing method steps are simpleOrganic chemistryAntineoplastic agentsPhenacylHydrogen
The invention relates to a pemetrexed-N,N-dibenzylethylenediamine salt and a preparation method thereof. The chemical name of the pemetrexed-N,N-dibenzylethylenediamine salt is N-[4-[2-(2-amino-4,7-dihydro-4-oxo-1H-pyrrolo[2,3-d]-pyrimidyl-5-yl)ethyl]benzoyl]-L-glutamic acid-N,N-dibenzylethylenediamine salt. The pemetrexed-N,N-dibenzylethylenediamine salt has favorable stability, can exist in the form of an anhydrous substance or hydrate. The pemetrexed-N,N-dibenzylethylenediamine salt is not reported in the prior art, thereby providing new options for research of pemetrexed preparation formulations. The preparation method has the advantage of simple and reasonable steps. The HPLC (high performance liquid chromatography) of the obtained product is greater than or equal to 99.70%, the single impurity content is less than 0.1%, and the total mol yield is up to 75-80%.
Owner:NINGBO MENOVO PHARMA
Application of palladium/active carbon catalyst in synthesizing N,N'-dibenzylethylenediamine
ActiveCN102179245BIncrease profitOvercome the disadvantage of producing a large amount of waste acidOrganic compound preparationAmino compound preparationEthylenediamineBenzyl-EDTA
Owner:嘉善县国创新能源研究院
Method for preparing cephapirin benzathine
The invention discloses a new method for preparing cephapirin benzathine by a one-pot method, relating to the field of chemical drug synthesis. The method comprises the following steps of: taking acetyl bromide 7-ACA as raw materials; in a solvent, in the presence of organic alkali, reacting the acetyl bromide 7-ACA with 4-pyridinethiols to obtain solid cefapirin acid; and then adding the organicalkali in the reaction liquid, dissolving the cefapirin acid as salt, and simultaneously and unnecessarily adding a reductant which is sodium thiosulfate, sodium hydrogensulfite or vitamin C; and then adding a reagent A in the reaction liquid, reacting the cefapirin acid salt with the reagent A at 0-50 DEG C for 0.1-20 hours to obtain the cephapirin benzathine, wherein the reagent A is dibezylethylenediamine diacetate acetate or dibezylethylenediamine diacetate. The method solves the problems that a product is easily decomposed, color is easily deepened in the process of preparing cefapirin sodium salt, and the like. The invention is simplified in steps, easy to operate and suitable for industrialized production, and the quality of the product accord with the quality standard of USP29.
Owner:GUANGZHOU BAIYUNSHAN PHARM CO LTD
A kind of method for preparing cefanixime dibenzylethylenediamine salt
The invention discloses a method for preparing cefnicil dibenzyl ethylenediamine salt, comprising A. acylation reaction: in a pure water system, adding 7-amino-3-(1-methanesulfonyl-1H-tetrazole -5-yl-thiomethyl)-cephem-2-carboxylic acid, add dilute ammonia water to dissolve it, then add a phase transfer catalyst, and dropwise add D-(-)-formylmandelic acid chloride and dilute ammonia water to control pH reaction to obtain an aqueous solution of formyl cefcinib acid; B. Deformylation: the aqueous solution of formyl cefcinid acid obtained in step A is heated to 25-35 ° C, and an acid solution is added to carry out hydrolysis reaction for 3-9 hours, and the hydrolysis is complete Then obtain an aqueous solution of cefcinic acid; C. salify: add N,N-dibenzylethylenediaminediacetic acid solution to the aqueous solution of cefcinic acid in step B, and stir and crystallize to obtain high-purity cefoxinic acid dibenzyl Ethylenediamine salt. The invention realizes emission reduction from the source, environmental protection, simple operation, and greatly reduces the production cost, and produces good economic and social benefits.
Owner:NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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