Preparation method of cefuroxime acid

A technology of cefuroxime acid and cefuroxime sodium, which is applied in the field of medicine, can solve the problems of high production cost, and achieve the effects of less impurities, easy operation and good stability

Active Publication Date: 2021-05-04
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation method of cefuroxime acid
  • Preparation method of cefuroxime acid
  • Preparation method of cefuroxime acid

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[0035] A preparation method of cefuroxime acid, characterized in that: using unqualified cefuroxime sodium as a raw material, put it into a dissolving agent and stir to dissolve it, then add an adsorbent to stir, after filtering, use an acidic reagent to crystallize to obtain cefuroxime bitter.

[0036] The quality index of cefuroxime sodium satisfies any one or a combination of total impurity ≤ 5.0%, maximum single impurity ≤ 2.0%, or solution color ≤ No. 7.

[0037] Including the following steps:

[0038] A. prepare mixed solution, control temperature, drop into unqualified cefuroxime sodium product, stir and dissolve to dissolve clear, obtain cefuroxime sodium solution liquid;

[0039] The mixed solution is selected from the combination of methanol, Virahol, acetonitrile and water; the volume and water ratio of each organic solvent in the mixed solution is 1:1:2; The gram-to-weight ratio is 20-30:1, and the temperature is controlled at 10-15°C during stirring.

[0040]B....

Embodiment 1

[0047] Add 100mL of methanol-isopropanol-water mixed solution into the dissolution tank, start stirring, control the temperature at 10°C, add 5 g of crude cefuroxime sodium, stir to dissolve, add 1 g of activated carbon loaded with 10% phosphoric acid, and check the pH value in the tank. When the pH drops to 4.5, filter, add 30% phosphoric acid to the filtrate dropwise to pH 3.6, add 0.15g cefuroxime acid, grow the crystal for 1 hour, continue to add 30% phosphoric acid dropwise until the pH is 1.9, stop, cool down to 5°C, filter and crystallize liquid, washed the wet powder with 15mL of acetone ethanol (3:1), placed in a decompression drying oven at 30°C and dried until the water content was qualified, and 4.61g of cefuroxime acid product was obtained.

Embodiment 2~4

[0049] Embodiments 2-4 have the same production process steps as in Embodiment 1, the difference is the selection of process parameters, as shown in Table 1 below.

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Abstract

The invention discloses a preparation method of cefuroxime acid, and belongs to the field of preparation of medical intermediates. The preparation method comprises the following steps: taking a cefuroxime sodium crude product as a raw material, adding into a dissolving agent, stirring, dissolving, adding an adsorbent, stirring, filtering, and crystallizing by using an acidic reagent to obtain the cefuroxime acid. The prepared cefuroxime acid has the advantages of high content, few impurities and good stability, and the preparation method is simple, energy-saving, environment-friendly and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a recovery and preparation method of cephalosporins, more specifically, to a one-step recovery and preparation method of cefuroxime sodium. Background technique [0002] Cefuroxime sodium is a semi-synthetic second-generation cephalosporin, which is effective against Staphylococcus aureus, Streptococcus, meningococcus, influenza bacillus, Klebsiella, Escherichia coli, Proteus mirabilis, Salmonella, Shigella, etc. Has a high antibacterial effect. This product can resist β-lactamase and is effective against penicillin-resistant Staphylococcus aureus. Clinically, it is mainly used for respiratory tract infection, pyelonephritis, urinary tract infection and bone, joint, ear, nose and throat, soft tissue infection caused by sensitive bacteria. This product has a sufficient amount to enter the cerebrospinal fluid during meningitis, and has a significant effect on meningitis caused by ...

Claims

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Application Information

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IPC IPC(8): C07D501/12C07D501/34
CPCC07D501/12C07D501/34
Inventor 任峰胡利敏贾全刘树斌田洪年孙玉双魏宝军乔俊华杨梦德贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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