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Cefoxitin sodium, preparation method and uses thereof

A technology of cefoxitin sodium and cefoxitin acid, applied in the field of its preparation and cefoxitin sodium, can solve the problems of cefoxitin sodium stability hidden danger, difficult to form stable crystal form, loss of washing and impurity removal effect, etc. , to achieve the effect of high solvent recovery efficiency, easy filtration and drying, and good stability

Active Publication Date: 2016-02-10
HAIKOU PHARMA FACTORY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because cefoxitin sodium is insoluble in organic solvents such as acetone, less cefoxitin sodium will be separated out when it is generated, and crystals will be separated out while generating the product, which is commonly referred to as reaction crystallization, and cefoxitin sodium is useful in this crystallization method Larger solvent wrapping and impurity wrapping, it is difficult to form a stable crystal form, especially a large amount of solvent wrapping (solvation), the liquid-solid ratio is small; in the post-treatment, the mother liquor is not easy to penetrate, the product adsorbs the mother liquor seriously, and the washing solvent is not easy to filter, It also cannot effectively exchange and remove the original reaction mother liquor; there are many residual solvents, which lose the effect of washing and removing impurities; the residual solvents usually dissolve a small amount of impurities, and the residual solvents can only be removed by high-temperature vacuum drying. Part is bound to stay and be brought into the product, which leaves a hidden danger for the stability of cefoxitin sodium

Method used

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  • Cefoxitin sodium, preparation method and uses thereof
  • Cefoxitin sodium, preparation method and uses thereof
  • Cefoxitin sodium, preparation method and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] In a 1000ml three-necked flask, add 15g of sodium carbonate, 0.2g of hydrosulfite, add 150g of water for injection and stir to dissolve, add 100g of cefoxitin acid, stir and dissolve at 25°C, add 5g of activated carbon for decolorization for 20 minutes, filter, and add the filtrate to In a 2000ml three-neck flask, control the temperature at 20-25°C, add 700ml of ethanol, the solution is slightly cloudy, continue to stir until the solution becomes dark and cloudy, until a small amount of crystals are precipitated, the turbidity becomes shallow, and a large number of crystals are precipitated. Cool to 5 -10°C, add 1000ml of ethanol again after half an hour. Keep warm for half an hour, filter, wash with a small amount of ethanol, drain, wet weight 125g at 40°C, and dry in vacuum for 2 hours to obtain 94.5g dry product of cefoxitin sodium.

Embodiment 2

[0075] In a 1000ml three-necked flask, add 40g of sodium isooctanoate and 0.2g of sodium hydrosulfite, add 150ml of water for injection and stir to dissolve, add 100g of cefoxitin acid, stir and dissolve at 25°C, add 5g of activated carbon for decolorization for 20 minutes, filter, and add the filtrate to Put it into a 2000ml three-neck flask, control the temperature at 20-25°C, add 700ml of isopropanol, the solution is slightly cloudy, and continue to stir until the solution becomes dark and cloudy, until a small amount of crystals precipitate out, the turbidity becomes shallow, and a large number of crystals precipitate out. Cool to 5-10°C, add 1000ml isopropanol again half an hour later. Keep warm for half an hour, filter, wash with a small amount of isopropanol, and drain to dryness. The wet weight is 125g, and vacuum-dried at 40°C for 2 hours to obtain 97.6g of dry cefoxitin sodium.

Embodiment 3

[0077] In a 1000ml three-neck flask, add 50g of 80% sodium lactate, 0.2g of sodium lactate, add 150ml of water for injection and stir to dissolve, add 100g of cefoxitin acid, stir and dissolve at 25°C, add 5g of activated carbon for decolorization for 20 minutes, filter, and add the filtrate to 2000ml In the three-neck flask, control the temperature at 20-25°C, add 700ml of propanol, the solution is slightly cloudy, continue to stir until the solution becomes dark and cloudy, until a small amount of crystals are precipitated, the turbidity becomes shallow, and a large number of crystals are precipitated. Cool to 5 -10°C, after half an hour, 1000 ml of propanol was added again. Insulate for half an hour, filter, wash with a small amount of propanol, drain, wet weight 125g, and vacuum dry at 40°C for 2 hours to obtain 96.8g dry product of cefoxitin sodium.

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Abstract

According to the present invention, on the process basis of the conventional cefoxitin sodium preparation method using a methanol and acetone mixing solvent or similar mixing solvent to carry out reaction crystallization, C1-C4 alkanol or tetrahydrofuran is adopted as a precipitating agent, and solvent crystallization is performed to prepare cefoxitin sodium; the obtained cefoxitin sodium has characteristics of good crystal form uniformity, good fluidity, stable quality, easy filtration, and easy drying; and the method is suitable for industrial production.

Description

technical field [0001] The present invention relates to cefoxitin sodium, its preparation method and application, especially unsolvated coupled cefoxitin sodium, its preparation method and application. Background technique [0002] Cefoxitin sodium belongs to β-lactam antibiotics. Because the 7-methoxy group in its structure is highly resistant to β-lactamase, it has outstanding antibacterial effect and is an excellent second-generation methoxycephalosporin. Cefoxitin sodium not only has strong antibacterial activity against Gram-negative bacteria, but also has strong antibacterial activity against Gram-negative bacteria, and has a good curative effect on mixed infections. Due to the short half-life of cefoxitin sodium, the half-life is only 40 minutes when given by injection, so it can be used in the delivery process of pregnant women. There is almost no residue in the milk of the parturient, and it has little impact on infants and young children. It is the first choice for...

Claims

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Application Information

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IPC IPC(8): C07D501/57C07D501/04C07D501/12A61K31/546A61P31/00A61P31/02
Inventor 白智全沙莹张志兰吴建军
Owner HAIKOU PHARMA FACTORY
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