A kind of method for preparing cefanixime dibenzylethylenediamine salt

A technology of dibenzylethylenediamine salt and dibenzylethylenediamine, which is applied in the field of preparation of dibenzylethylenediamine salt of cefonicil, and can solve the problem of low yield, low utilization rate of equipment and poor quality and other problems, to achieve high yield, less impurities, and reduce production costs

Active Publication Date: 2018-02-13
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved in the present invention is to provide a method for the preparation of cefanixidibenzylethylenediamine salt with simple operation, environmental protection, high yield and high purity. The method is a "one-pot method" and solves the problem Existing technologies use a large amount of organic solvents, low utilization rate of equipment, low yield and poor quality

Method used

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  • A kind of method for preparing cefanixime dibenzylethylenediamine salt
  • A kind of method for preparing cefanixime dibenzylethylenediamine salt
  • A kind of method for preparing cefanixime dibenzylethylenediamine salt

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Embodiment 1

[0054] A. Acylation reaction: Add 100kg of raw material I in 600L of purified water, then add dilute ammonia water and stir until it is completely dissolved, cool down in -7°C water, and add 8g of tetrabutylammonium bromide after the temperature of the reaction system drops to 3°C. Feed 53kg of raw material II, and at the same time feed dilute ammonia water to control the pH of the reaction system to be 6.0-8.0, and the reaction time is 0.5 hours to obtain an aqueous solution of formylcefocinic acid, and the reaction temperature is controlled at 0-5°C during the whole process;

[0055] B. Deformylation reaction: Add 25L of 37% (mass fraction) concentrated hydrochloric acid to the aqueous solution of formylcefocinic acid obtained in step A, the solution is warmed up to 35°C, and the hydrolysis reaction is carried out for 3 hours to obtain the aqueous solution of cefuroxime acid; Then lower the temperature to 25°C, add 10kg of activated carbon for decolorization for 30 minutes, f...

Embodiment 2

[0058] A. Acylation reaction: In 600L of purified water, add 100kg of raw material I, then add dilute ammonia water and stir until it is completely dissolved, cool down in -7°C water, and add 340g of tetrabutylammonium chloride after the temperature of the reaction system drops to 4°C. Feed 53 kg of raw material II, and at the same time feed dilute ammonia water to control the pH to 6.0-8.0, and the reaction time is 2 hours to obtain formylcefocinic acid aqueous solution, and the reaction temperature is controlled at 0-5°C during the whole process;

[0059] B. Deformylation reaction: Add 34L of 85% (mass fraction) phosphoric acid to the aqueous solution of formylcefocinic acid obtained in step A, the solution is warmed up to 25°C, and the hydrolysis reaction is carried out for 9 hours to obtain the aqueous solution of cefuroxime acid; Add 10kg of activated carbon for decolorization for 30 minutes, filter, wash with a small amount of water, and combine the filtrates;

[0060] C...

Embodiment 3

[0062] A. Acylation reaction: In 600L of purified water, add 100k of raw material I, then add dilute ammonia and stir until it is completely dissolved, cool down in -7°C water, add 50g of TEBA after the temperature of the reaction system drops to 0°C, and then add 53kg of raw material II, At the same time, dilute ammonia water was added to control the pH to 6.0-8.0, and the reaction time was 1 hour to obtain an aqueous solution of formylcefocinic acid, and the reaction temperature was controlled at 0-5°C during the whole process;

[0063] B. Deformylation reaction: add the mixed acid of 20L37% (mass fraction) concentrated hydrochloric acid and 10L85% (mass fraction) phosphoric acid in the aqueous solution of formyl cefocinic acid that step A obtains, solution is warming up to 30 ℃, hydrolysis reaction After 7 hours, an aqueous solution of cefocinic acid was obtained; 10 kg of activated carbon was added for decolorization for 30 min, filtered, washed with a small amount of water...

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Abstract

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.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for preparing a drug intermediate, in particular to a method for preparing cefanisidine dibenzylethylenediamine salt. Background technique [0002] Cefonicid Sodium (Cefonicid Sodium, CAS No.: 61270-78-8), its chemical name is: (6R, 7R)-7-(R)-hydroxyphenylacetamido-3-1-(sulfonic acid methyl -1H-tetrazol-5-yl)thiomethyl-8-oxo-5thia-1-azabicyclo4.2.0oct-2-ene-2-carboxylic acid disodium salt, second generation Broad-spectrum, long-acting cephalosporin antibiotics, which produce antibacterial activity by inhibiting the synthesis of bacterial cell walls, have antibacterial effects on Gram-positive and negative bacteria and some anaerobic bacteria, are stable to most β-lactamases, and are suitable for sensitive Bacteria can cause lower respiratory tract infection, urinary tract infection, sepsis, skin and soft tissue infection, bone and joint infection, and can also be used to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36C07D501/04C07C211/27C07C209/68
CPCC07D501/04C07D501/36
Inventor 谭清钟魏青杰胡利敏张锁庆李惠芬任峰郭玉聪刘树斌杨梦思杨庆江张鑫吴士军
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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