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Method for recovering cefuroxime acid from cefuroxime acid waste residue liquid

A technology of cefuroxime acid and waste residue liquid, which is applied in the direction of organic chemistry, can solve the problems of low production cost, and achieve the effects of low production cost, simple reaction process and improved purity

Active Publication Date: 2021-03-30
山东金城昆仑药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of this invention is to provide a method for reclaiming cefuroxime acid from cefuroxime acid waste residue liquid, directly converting trans isomer by-products into cis products, which not only solves the environmental protection problems caused by waste residue, but also improves the product quality. The yield is high, and no other reaction raw materials are consumed in the middle, and the production cost is low

Method used

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  • Method for recovering cefuroxime acid from cefuroxime acid waste residue liquid
  • Method for recovering cefuroxime acid from cefuroxime acid waste residue liquid
  • Method for recovering cefuroxime acid from cefuroxime acid waste residue liquid

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preparation example Construction

[0029] The preparation method of polymer supported catalyst in the embodiment is as follows:

[0030] Immerse 5-6g of polymer material in 50ml of absolute ethanol for 2-3 hours, under the protection of nitrogen, add 2-3g of Lewis acid to reflux for 2-2.5 hours, cool to room temperature, filter with suction to remove the solvent, and wash the filter cake with acetone , drying at room temperature, prepared. Where the Lewis acid is TiCl 4 , AlCl 3 or BBr 3 ; The polymer material is one or both of polyvinyl chloride or polystyrene.

Embodiment 1

[0032] 40g cefuroxime acid waste residue liquid (HPLC detection trans isomer peak area ratio is 6%) was dissolved in 200ml water, filtered to obtain a clear solution, adding polymer-loaded catalyst PVC-AlCl in the clear solution 3 , PVC-AlCl 3 % of the total mass of the clarified solution, stirred and reacted at 20° C. for 5 h, and distilled under reduced pressure to obtain 15 g of cefuroxime acid product. The cefuroxime acid product is detected by HPLC, and its chromatogram is as follows: figure 1 Shown: the peak area ratio of the trans isomer is 0.131%. Based on the total mass of cefuroxime acid waste residue liquid, the yield of cefuroxime acid product was 37.5%, and the purity was 99.441%.

Embodiment 2～7

[0034] The process of reclaiming cefuroxime acid from the cefuroxime acid waste residue liquid is the same as in Example 1, adjusting the reaction temperature, the reaction time, the consumption of the cefuroxime acid waste residue liquid, the type and amount of the solvent, the type and the amount of the polymer-loaded catalyst, specifically The data are shown in Table 1.

[0035] The data sheet in the embodiment 2~7 of table 1

[0036]

[0037]

[0038] The cefuroxime acid products in Examples 1-7 were tested for quality. The products obtained in Examples 1-7 were all white crystalline powders, all of which met the product requirements, and the content of trans isomers was all less than 0.5%.

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Abstract

The invention relates to the technical field of medicine synthesis, in particular to a method for recovering cefuroxime acid from cefuroxime acid waste residue liquid. The method comprises the steps of: dissolving the cefuroxime acid waste residue liquid in a solvent, filtering, adding a polymer supported catalyst into the filtrate, reacting, and carrying out reduced pressure distillation to obtain the cefuroxime acid. According to the invention, trans-isomer byproducts are directly converted into cis-products, so that the environmental protection problem caused by waste residues is solved, the product yield is increased, the cis-products in the reaction process are not damaged and can be completely recycled by a reaction system, the reaction process is simple, other reaction raw materialsare not consumed in the process, the process is simple, and the production cost is low.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical synthesis, in particular to a method for recovering cefuroxime acid from cefuroxime acid waste residue liquid. Background technique [0002] Cefuroxime acid is an intermediate in the synthesis of the second-generation cephalosporin antibiotics cefuroxime axetil and cefuroxime sodium. Cefuroxime antibiotics have a broad-spectrum antibacterial effect and a wide range of applications. They can be used for respiratory tract infections, ENT infections, urinary system infections, skin and soft tissue infections, bone and joint infections, gonorrhea, including sepsis and meninges caused by sensitive bacteria. and other infections, it is the leading variety of second-generation cephalosporin antibiotics. [0003] Chinese patent CN101928292A discloses a preparation method of cefuroxime acid. The method is to use 7-aminocephalosporanic acid (7-ACA) and methoxyiminofuran acetate as raw materials for...

Claims

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Application Information

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IPC IPC(8): C07D501/34C07D501/12C07D501/04
CPCC07D501/34C07D501/12C07D501/04
Inventor 付凯孙铎代建建
Owner 山东金城昆仑药业有限公司
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