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Preparation method for cefazedone sodium with low water content

A technology of cefazedone sodium and water content, which is applied in the field of medicine, can solve the problems of low drying efficiency and difficulty in reproducing product moisture control, and achieve the effects of long crystallization time, ensuring reproducible consistency, and reducing water content

Active Publication Date: 2015-03-04
天津新丰制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in CN 101584671A, the cefazedone sodium solid is dissolved in water, decolorized and filtered by activated carbon, acetone is added to the filtrate to crystallize, and the crystals are filtered and dried to obtain cefazedone sodium crystals. The drying method controls moisture, and there are problems such as low drying efficiency and difficulty in reproducing moisture control of different batches of products.

Method used

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  • Preparation method for cefazedone sodium with low water content
  • Preparation method for cefazedone sodium with low water content

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A kind of preparation method of low water content cefazedone sodium, the steps are as follows:

[0035] (1) Liquid dosing: the reaction kettle, filter and utensils used are carried out aseptic treatment, 2000g (3.65mol) cefazedone, 296g (5.48mol) sodium methylate and 20.36L anhydrous methanol are added in the 50L reaction kettle, Stir to dissolve completely, and cool the reaction solution to 10-30°C;

[0036] (2) Decolorization: Then add 80g of activated carbon, stir and adsorb for 30 minutes, decarbonize through titanium rod filtration, and the filtrate is further decarburized and sterilized through a 0.22 μm microporous membrane; and wash the place where the reaction solution passes through with anhydrous methanol, and combine the filtrate and washing liquid and keep the temperature at 15-25°C, and use a filter membrane with a molecular cut-off of 1000 Daltons for ultrafiltration;

[0037] (3) Crystallization: The filtrate was transferred to a 50L crystallization tan...

Embodiment 2

[0040] A kind of preparation method of low water content cefazedone sodium, the steps are as follows:

[0041] (1) Dosing: carry out aseptic treatment to used reactor, filter, utensil, 2100g (3.83mol) cefoxizone, 228g (4.21mol) sodium methylate and 21.37L anhydrous methanol are added in 50L reactor, Stir to dissolve completely, and cool the reaction solution to 10-30°C;

[0042] (2) Decolorization: Then add 73.5g of activated carbon, stir and adsorb for 30 minutes, decarbonize through titanium rod filtration, and further decarburize and sterilize the filtrate through a 0.22 μm microporous membrane; wash the place where the reaction solution passes through with anhydrous methanol, combine and filter liquid and washing liquid and keep the temperature at 15-25°C, and use a filter membrane with a molecular cut-off of 1000 Daltons for ultrafiltration;

[0043] (3) Crystallization: The filtrate was transferred to a 50L crystallization tank in a 10,000-class local clean area, 26.75L...

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Abstract

The invention relates to a preparation method for cefazedone sodium with low water content. The method includes the following steps: performing salifying: placing cefazedone and sodium methoxide into dried methyl alcohol for a salifying reaction, and cooling a reaction solution to 10-30DEG C when the cefazedone is completely dissolved; decoloration: adding activated carbon into the reaction solution, stirring for decoloration, filtering out the activated carbon, and then performing ultrafiltration; crystallization; and drying: filtering and washing filter cake to obtain the cefazedone sodium with low water content. According to the method, the cefazedone and sodium methoxide are placed into the dried methyl alcohol for the salifying reaction so as to obtain cefazedone sodium with low water content, and simultaneously, ultrafiltration and ultrasonic crystallization technologies are adopted to produce the cefazedone sodium which is low in water content, few in impurities, uniform in particles, good in liquidity and high in stability.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a preparation method of cefazedone sodium with low water content. Background technique [0002] Cefoxitone Sodium is the first generation cephalosporin researched and developed by E.Merck, Darmstadt laboratory. In 1979, E.Merck was the first to go on the market in Germany, and then in its surrounding areas and South Korea, Romania, Bulgaria, Taiwan, etc. Listed in countries and regions, its English name is Cefazedone Sodium; chemical name is (6R,7R)-7-(2-(3,5-dichloro-4-oxo-1(4H)-pyridyl)acetamido) -3-(((5-methyl-1,3,4-thiodiazol-2-yl)thio)methyl)-8-oxo-5-thia-1-azabicyclo[4.2.0 ] Sodium oct-2-ene-2-carboxylate. [0003] Its chemical structural formula is: [0004] [0005] The above structure of cefoxitone sodium is similar to that of cefazolin sodium, both of which are β-lactam antibiotics. [0006] Cefoxizone sodium against Staphylococcus aureus, coagulase-negative sta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36C07D501/04C07D501/12
Inventor 李章才高朝阳刘文玖林澜王春玲许龙哲崔连泉
Owner 天津新丰制药有限公司
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