44 results about "Benzyl-EDTA" patented technology

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

The invention discloses preparation methods of dibenzyl ethylidenediamine and acetate thereof, which relates to the preparation methods of compounds, wherein the preparation method of the dibenzyl ethylidenediamine comprises the following steps: benzaldehyde reacts with ethylidenediamine for dehydrating so as to obtain Schiff base under the condition of existence of alcohol; and the Schiff base is reduced by hydrogen to obtain the dibenzyl ethylidenediamine under the condition of existence of alcohol and a catalyst. The preparation method of the acetate of the dibenzyl ethylidenediamine comprises the following step: glacial acetic acid is directly added to the alcoholic solution of the dibenzyl ethylidenediamine to be salified to obtain the acetate of the dibenzyl ethylidenediamine. The invention has simple process, short time, high product quality, low environment pollution, high conversion rate and low cost.

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.

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.

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.

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.

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.

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.

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.

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%.