Method for refining cefonicid dibenzyl ethylenediamine salts

A technology of cefnixime dibenzylethylenediamine salt and cefdonizil salt, which is applied in the field of refining cefnixime intermediates, can solve the problem that cannot be used in the preparation of cefnixime sodium powder for injection, cefnixime sodium Benzyl ethylenediamine salt has deep color grade and unqualified quality of cefanixime sodium finished product, so as to achieve the effect of easy control of the production process, no by-product formation, and less impurities

Active Publication Date: 2019-01-18
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing cefanisidine dibenzylethylenediamine salt, problems such as the relatively large amount of impurities remaining in the acylation reaction and the excessively high hydrolysis temperature lead to darker color grades and imp...

Method used

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  • Method for refining cefonicid dibenzyl ethylenediamine salts
  • Method for refining cefonicid dibenzyl ethylenediamine salts
  • Method for refining cefonicid dibenzyl ethylenediamine salts

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preparation example Construction

[0030] The preparation method comprises the following steps:

[0031] A. Resin ion exchange: first add cation exchange resin to the lysate, then add the crude product of cefanisil salt, stir at 0-20°C until the crude product of cefanisil salt is completely dissolved, and filter out the resin after stirring for 2-6 hours. Then the aqueous phase is separated from the organic phase, and the aqueous phase is retained for decolorization treatment, and the filtered resin is soaked and washed with water 0.5 to 2 times the quality of the crude product of cefonixime salt to obtain lotion A;

[0032] The cation exchange resin is any one of Amberlyst 15, Amberlite IR-120, Duolite ES-280, Themax T-63 or Themax T-54, and the mass ratio of the cation exchange resin to the crude product of cefanixime salt is 2 to 5 :1;

[0033] Described eluent is the mixing of water and organic solvent A, and organic solvent A is the mixing of any one or several in methylene dichloride, ethyl acetate, carb...

Embodiment 1

[0043] A kind of refining method of cefanixime dibenzylethylenediamine salt, the crude product of cefanixime dibenzylethylenediamine salt is ion-exchanged with a resin and decolorized with a decolorizing agent, and then undergoes a salt-forming reaction with a transamination agent, After crystallization with a precipitating agent, the refined cefanisidine dibenzylethylenediamine salt is obtained.

[0044] The preparation method comprises the following steps:

[0045] A. Resin ion exchange: Add 10ml of ethyl acetate and 60ml of purified water into the reaction tank, then add 40g of Amberlyst 15 macroporous cation exchange resin, control the temperature at 0°C and stir, add 20g of cefanixime dibenzylethylenediamine salt For the crude product, stir at 0°C until the crude product of cefanixime dibenzylethylenediamine salt is completely dissolved; after stirring for 2 hours, filter out the resin, statically separate the phases, keep the lower aqueous phase for decolorization treatm...

Embodiment 2～5

[0049] Embodiments 2-5 are the same as the process steps in embodiment 1, the difference is the selection of process parameters, as shown in Table 1 below.

[0050] Table 1

[0051]

[0052]

[0053]

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Abstract

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.

Description

technical field [0001] The invention relates to cephalosporins, in particular to a method for refining a cefnixime intermediate, and belongs to the technical field of medicine. Background technique [0002] The chemical name of cefnixime sodium is (6R,7R)-7-[(R)-α-hydroxyphenylacetamido]-8-oxo-3-[[[1-sulfonic acid methyl-1H-tetrazole -5-yl]thio]methyl]-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid disodium salt, white or off-white powder or crystalline Powder, easily soluble in water, very slightly soluble in methanol and ethanol, almost insoluble in ether, its structural formula is as follows: [0003] [0004] Cefnixime sodium is a second-generation cephalosporin. It produces antibacterial activity by inhibiting the synthesis of bacterial cell walls. It has antibacterial effects on Gram-positive and negative bacteria and some anaerobic bacteria. It is stable to most β-lactamases and is applicable Sensitive bacteria cause lower respiratory tract infection, urin...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12C07C211/27C07C209/00
CPCC07D501/12C07D501/36
Inventor 任峰石春利李庆伟贾全张锁庆田洪年刘树斌魏宝军于亚南
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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