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A purifying method of a novel antibiotic compound

A purification method and antibiotic technology, applied in the field of medicine, can solve the problems of low volatility, easy residue and high product impurity content, and achieve the effects of reducing the generation of degradation impurities, reducing the impurity content of the product and improving the product yield

Active Publication Date: 2014-10-29
SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD +2
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The fine cefazedone sodium obtained in the prior art has problems such as high water content and high impurity content, and the preparation process also has problems such as complicated operation, high cost, low yield, and large pollution
[0005] For example, in CN101584671A, the cefazedone sodium solid is dissolved in water, and after activated carbon decolorization and filtration, acetone crystallization is added in the filtrate, and the crystals are filtered and dried to obtain cefazedone sodium crystals. method to control moisture, there are problems such as low drying efficiency and difficulty in reproducing moisture control of different batches of products
[0006] CN102924482A discloses a kind of preparation method of low water content cefazedone sodium, has following shortcoming: (1) adopt sodium methylate as salt-forming solvent, alkalinity is too strong, makes cefazedone β-lactam ring easy to be destroyed, impurity High content, strong corrosiveness, and large pollution; (2) using isopropanol as a crystallization solvent, with a high boiling point and low volatility, which is easy to remain in the product and increase the impurity content; (3) ultrasonic crystallization is used in the crystallization process Oscillatory seeding method produces seeds
This preparation method is loaded down with trivial details operation, high to equipment requirement, pollution is big, cost is also high, and the obtained product impurity content is high, and yield is low; (4) preparation method yield is low, only 85%

Method used

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  • A purifying method of a novel antibiotic compound
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  • A purifying method of a novel antibiotic compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of refining method of novel antibiotic compound cefazedone sodium, the steps are as follows:

[0033] (1) Salt formation: Aseptically treat the reaction kettle, filter, and utensils used, and add 1096.9g (2mol) cefazinone, 398.9g (2.4mol) sodium isooctanoate and 6.58L anhydrous methanol to a 50L reaction kettle , stir to dissolve completely, and control the temperature at 15-35°C;

[0034] (2) Decolorization: Add 11g of activated carbon into the reaction solution, stir and absorb for 30 minutes, filter the titanium rod for decarbonization, and pass the filtrate through a 0.22 μm microporous membrane for further decarbonization and sterilization, and keep the temperature of the filtrate at 10-30°C;

[0035] (3) Crystallization: The filtrate is transferred to a 50L crystallization tank in a local clean area of ​​10,000 grades, and a mixed solvent of 5.86L acetone and 2.93L ethyl acetate is added to the filtered filtrate, and the temperature is controlled at 15-20°C...

Embodiment 2

[0038] A kind of refining method of novel antibiotic compound cefazedone sodium, the steps are as follows:

[0039] (1) Salt formation: Aseptically treat the reaction kettle, filter and utensils used, and add 1096.9g (2mol) cefazinone, 465.33g (2.8mol) sodium isooctanoate and 8.78L anhydrous methanol to a 50L reaction kettle , stir to dissolve completely, and control the temperature at 15-35°C;

[0040] (2) Decolorization: Add 22g of activated carbon into the reaction solution, stir and absorb for 30 minutes, filter the titanium rod for decarbonization, and pass the filtrate through a 0.22μm microporous membrane for further decarbonization and sterilization, and keep the temperature of the filtrate at 10-30°C;

[0041] (3) Crystallization: The filtrate is transferred to a 50L crystallization tank in a local clean area of ​​10,000 grades, and a mixed solvent of 7.32L acetone and 3.66L ethyl acetate is added to the filtered filtrate, and the temperature is controlled at 15-20°C....

Embodiment 3

[0044] A kind of refining method of novel antibiotic compound cefazedone sodium, the steps are as follows:

[0045](1) Salt formation: Aseptically treat the reaction kettle, filter and utensils used, and add 1096.9g (2mol) cefazedone, 531.8g (3.2mol) sodium acetate and 10.97L anhydrous methanol into the 50L reaction kettle , stir to dissolve completely, and control the temperature at 15-35°C;

[0046] (2) Decolorization: Add 32.9g of activated carbon into the reaction solution, stir and adsorb for 30 minutes, filter the titanium rod for decarbonization, and pass the filtrate through a 0.22μm microporous membrane for further decarbonization and sterilization, and keep the temperature of the filtrate at 10-30°C;

[0047] (3) Crystallization: The filtrate is transferred to a 50L crystallization tank in a local clean area of ​​10,000 grades, and a mixed solvent of 8.78L acetone and 4.39L ethyl acetate is added to the filtered filtrate, and the temperature is controlled at 15-20°C....

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Abstract

The invention relates to a purifying method of a novel antibiotic compound. The method includes: (1) a step of salifying, namely a step of adding cefazedone and sodium isooctoate into absolute methanol and performing a salifying reaction until the cefazedone is fully dissolved, with the temperature being controlled at 15-35 DEG C; (2) a step of decoloring, namely a step of adding active carbon into the reaction solution, stirring, decoloring, filtering to remove the active carbon, maintaining the temperature of the filtrate at 10-30 DEG C, and filtering again; (3) a step of crystallizing, namely a step of adding a certain amount of acetone and ethyl acetate into the filtrate after the filtration, controlling the temperature at 15-20 DEG C, growing the grain for 1-2 h, then adding a certain amount of the acetone and the ethyl acetate, stirring for crystallization with the stirring speed being maintained at 80-120 r / min, controlling the temperature at 15-25 DEG C, and growing the grain for 2-4 h; and (4) a step of drying, namely a step of filtering, washing the filter cake, and drying to obtain a purified product of the cefazedone sodium. Compared with the prior art, the method has characteristics of simple operation, low cost, high yield, and largely reduced pollution. The purified product of the cefazedone sodium has characteristics of low water content, low purity content and high stability.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for refining a novel antibiotic compound, in particular to a method for refining a cefazedone sodium compound. Background technique [0002] Infectious diseases are a common and frequently-occurring disease in clinical practice. According to the report of the World Health Organization (WHO), the number of deaths from infectious diseases is as high as 33.3% of the total number of deaths from various causes. Cephalosporins are the most widely used first-line drugs in clinical practice. In recent years, due to the abuse of antibiotics, many "super bacteria" have emerged, and the problem of bacterial drug resistance has become increasingly serious. The "Administrative Measures for the Clinical Application of Antibacterial Drugs" officially implemented by the state restricts the clinical application of the third-generation and fourth-generation cephalosporins with strong alt...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12C07D501/04
CPCC07D501/04C07D501/12C07D501/36
Inventor 侯善波李晓峰宋丽丽
Owner SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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