Refining method of ceftizoxime sodium

A technology of cefizoxime sodium and a purification method, applied in the field of medicine, can solve the problems of many side reactions, low yield, complicated steps and the like, achieve high product yield and purity, improve total yield and purity, and reduce side reactions Effect

Active Publication Date: 2019-04-02
SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The preparation method of the prior art has cumbersome steps and many side reactions, and is not suitable for industrial production; or the yield is low, raw materials are wasted, and production costs are increased
In addition, in some cases, due to improper control...

Method used

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  • Refining method of ceftizoxime sodium
  • Refining method of ceftizoxime sodium
  • Refining method of ceftizoxime sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Synthesis of ceftizoxamic acid

[0023] Add 20.01g (0.1mol) of 7-ANCA, 150ml of dichloromethane, and 0.15mol of N,N-diisopropylethylamine to the reactor in order to stir and dissolve, control the temperature at 0-5°C, and add AE active ester dropwise 35.02g (0.1mol), after 15 minutes, add 0.05mol of 4-dimethylaminopyridine, keep the temperature condition unchanged, stir and react for 3-4h, after the reaction, add water at room temperature for layering, and organic The phases are separated, the aqueous phase is retained, and dichloromethane is added for washing, then activated carbon is added for decolorization, hydrochloric acid is added for crystallization, centrifugation, and drying obtains 33.02 g of ceftizoxamic acid, the product yield is 86%, the purity is 99.5%, and the maximum single hetero 0.08%, total miscellaneous 0.52%.

[0024] (2) Refining of Ceftizoxime Sodium

[0025] Add 33.02 g of ceftizoxime acid to 198 ml of water to dissolve, add concentrated h...

Embodiment 2

[0027] (1) Synthesis of ceftizoxamic acid

[0028] Add 20.02g (0.1mol) of 7-ANCA, 150ml of dichloromethane, and 0.15mol of triethylamine to the reactor in order to stir and dissolve, and control it at -5-0°C, add 38.52g (0.11mol) of AE active ester dropwise , after 15 minutes, add 0.05 mol of 4-dimethylaminopyridine, keep the temperature constant, and stir for 3-4 hours. After the reaction, add water at room temperature for layering, separate the organic phase, and keep the water phase, adding dichloromethane for washing, then adding activated carbon for decolorization, adding hydrochloric acid for crystallization, centrifuging, and drying to obtain 36.79 g of ceftizoxamic acid, with a yield of 96%, a purity of 99.7%, a maximum of 0.05% of impurities, and a total of 0.22% of impurities.

[0029] (2) Refining of Ceftizoxime Sodium

[0030] Add 36.79g of ceftizoxime acid to 221ml of water to dissolve, add concentrated hydrochloric acid to control the pH to 2.5, add 16.13g (0.19...

Embodiment 3

[0032] (1) Synthesis of ceftizoxamic acid

[0033] Add 20.02g (0.1mol) of 7-ANCA, 150ml of dichloromethane, and 0.15mol of triethylamine to the reactor in order to stir and dissolve, and control the condition of 5-10°C, add 42.01g (0.12mol) of AE active ester dropwise, Add in 15 minutes, keep the temperature condition unchanged, stir and react for 3-4h, after the reaction is over, add water at room temperature for layering, separate the organic phase, keep the water phase, add dichloromethane for washing, and then add activated carbon Decolorize, add hydrochloric acid to crystallize, centrifuge, and dry to obtain 31.84 g of ceftizoxime acid, with a yield of 83%, a purity of 99.6%, a maximum of 0.15% of impurities, and 0.39% of total impurities.

[0034] (2) Refining of Ceftizoxime Sodium

[0035] Add 31.84g of ceftizoxime acid to 191ml of water to dissolve, add concentrated hydrochloric acid to control the pH to 2, add 13.94g (0.166mol) of sodium bicarbonate, add 64ml of meth...

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Abstract

The invention discloses a refining method of ceftizoxime sodium. The refining method comprises the following steps: dissolving cefazoxime acid into water, adding concentrated hydrochloric acid to control the pH value after dissolution and clarification, adding sodium bicarbonate, adding an organic solvent, uniformly carrying out stirring, adding activated carbon for decoloration, carrying out filtering, controlling the temperature to be 15-20 DEG C, rapidly carrying out stirring at frequency of 30-40 HZ, adding acetone, carrying out cooling to 0-5 DEG C, controlling the stirring frequency to be 20 HZ, carrying out crystal growing for 1-2 hours, and carrying out drying to obtain a cefazoxime sodium fine product. According to the refining method disclosed by the invention, the purity of theobtained cefazoxime sodium can reach 99.9% or above, the content of total impurities and the content of a maximum single impurity are respectively controlled to be within 0.2% and 0.05%, the quality of the product is remarkably improved, the refining process is simple and convenient to operate, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicines, in particular to a method for refining ceftizoxime sodium. Background technique [0002] Ceftizoxime sodium, English name: Ceftizoxime Sodium, chemical name: (6R, 7R)-7-[(Z)-2-(2-amino-4-thiazolyl)-2-methoxyiminoacetamide Base]-8-oxo-5-thia-1-aminoheterobicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt, the structural formula is: [0003] [0004] Ceftizoxime sodium is the third-generation cephalosporin antibiotic first developed by Fujisawa Pharmaceutical Co., Ltd. in Japan. It was first listed in Japan in 1982 under the trade name Ceftizox. This product is a third-generation cephalosporin antibiotic. Its mechanism of action is to achieve bactericidal effect by inhibiting the biosynthesis of bacterial cell wall mucopeptides. It has the characteristics of broad-spectrum, high efficiency, enzyme resistance, low toxicity and can pass through the blood-brain barrier. It is stable against ...

Claims

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Application Information

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IPC IPC(8): C07D501/12C07D501/20
CPCC07D501/12C07D501/20
Inventor 孙松朱志强王奔
Owner SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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