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One-step recovery and preparation method of cefuroxime sodium

A technology of cefuroxime sodium and cefuroxime acid, which is applied in the field of medicine, can solve the problems of unsuitable storage, prolonged dissolution time, and long time, and achieve the effects of improving recovery work efficiency, good protection, and good product quality

Inactive Publication Date: 2011-12-28
GUANGZHOU BAIYUNSHAN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If it is not dried, first, it is not suitable for storage, and the color of the wet product of cefuroxime acid changes rapidly; second, it is not suitable for feeding and using, because the wet product of cefuroxime acid contains a large amount of water, which will bring a lot of water to the system for preparing cefuroxime sodium. Enter a large amount of water, affect the preparation of cefuroxime sodium
Therefore, the wet product of cefuroxime acid generally needs to be dried, and the drying process takes a long time. Generally, 100 kg of cefuroxime acid needs to be dried at 30-50 degrees for as long as 5-10 hours. During the drying process, cefuroxime acid is in a state of high temperature and high humidity, which will cause the color and impurities of cefuroxime acid to increase, and the quality of recovered cefuroxime sodium is not good
[0009] 2. Method 2 seems simple, and there is no drying process of adding acidic substances and cefuroxime acid in method 1. However, recrystallization of unqualified cefuroxime sodium in water and organic solvents often results in fine particles of cefuroxime sodium. Moreover, the impurities are not easy to remove, the product is not easy to dry, and the product quality and yield are not satisfactory
And above-mentioned two recovery methods all will use a large amount of water to carry out the dissolving of cefuroxime sodium, so the quality of the cefuroxime sodium that reclaims is often not good
If the dissolution time in industrial production is prolonged, the recovered cefuroxime sodium may even appear darker than the original cefuroxime sodium

Method used

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  • One-step recovery and preparation method of cefuroxime sodium

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Add 10 grams of unqualified cefuroxime sodium (color and luster is equal to yellow No. 7, content 92%) in 100ml 95% ethanol and 200ml acetone, add hydrochloric acid 1.3ml (form by adding 0.65ml of water 0.65ml of 36% hydrochloric acid), Incubate at 10-15°C for 2 hours, cefuroxime sodium is gradually converted into cefuroxime acid and dissolved in the reaction system; add 1 g of activated carbon, stir for 15 minutes to decolorize, filter, filter out the activated carbon, and use 20ml of ethanol for the filter cake Wash, and combine the filtrate and the carbon washing solution to obtain a cefuroxime acid solution.

[0031] 20~25 ℃, add the mixed solution of 6 grams of 60% sodium lactate and 75ml ethanol into the above-mentioned cefuroxime acid solution under stirring, after adding, continue to stir for 1 hour, filter, collect and wash the crystals with ethanol, the crystals are at 35 Vacuum drying at ~45°C gave 9.2 g of cefuroxime sodium with a yield of 92%. The obtained...

Embodiment 2

[0033]Add 10 grams of unqualified cefuroxime sodium (color equal to yellow No. 8, content 91%) into 300ml of methanol and 150ml of acetone, add 10ml of sulfuric acid (prepared from 1ml of 98% sulfuric acid and 9ml of water), 0-10 ℃ for 1 hour, cefuroxime sodium is gradually converted into cefuroxime acid and dissolved in the reaction system, 2 grams of activated carbon is added, stirred for 15 minutes, filtered, washed with 50ml of methanol, and the filtrate and carbon washing liquid are combined to obtain cephalosporin Furoic acid solution.

[0034] 0~15℃, add the mixed solution of 12.5 grams of 60% sodium lactate and 120ml of acetone into the above cefuroxime acid solution under stirring, after the addition, continue to stir for 4~5 hours, filter, collect and wash the crystals with acetone, the crystals are in Vacuum drying at 35-45°C gave 8.9 g of cefuroxime sodium with a yield of 89%. The color of the obtained cefuroxime sodium was detected according to the detection meth...

Embodiment 3

[0036] Add 10 grams of unqualified cefuroxime sodium (the clarity of cefuroxime sodium is greater than No. 2 turbidity standard solution, content 91%) in 80ml acetone and 20ml isopropanol, add hydrochloric acid 2.2ml (by 36% hydrochloric acid 1.1 ml and 1.1ml of water), and react at 40-50°C for 0.5 hours, cefuroxime sodium is gradually converted into cefuroxime acid and dissolved in the reaction system, add 0.1 g of activated carbon, stir for 15 minutes, filter, and use 20ml Wash with acetone, and combine the filtrate and the carbon washing liquid to obtain a cefuroxime acid solution.

[0037] 40~50℃, add 8 grams of sodium isooctanoate, 16ml of acetone and 1.6ml of water into the above cefuroxime acid solution under stirring, after the addition, continue to stir for 1 hour, filter, collect and wash the crystals with acetone, the crystals Vacuum drying at 35 to 45°C yielded 8.7 grams of cefuroxime sodium, with a yield of 87%, and the obtained cefuroxime sodium was detected by t...

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Abstract

The invention relates to a one-step recovery and preparation method of cefuroxime sodium. The method comprises: dispersing cefuroxime sodium in a water-containing or non-aqueous mixed solvent of alcohol and ketone, adding hydrochloric acid or sulfuric acid at a temperature of 0-50°C, and reacting for 0.5-3 hours, and cefuroxime sodium is gradually converted into cefuroxime Fuuroctanoic acid is dissolved in the reaction system, and the by-product sodium chloride or sodium sulfate generated simultaneously is insoluble in the reaction system; Then, activated carbon is added for decolorization, filtered, and the by-product and activated carbon are filtered to obtain the cefuroxime acid solution; the obtained Cefuroxime sodium solution is mixed with sodium lactate or sodium isooctanoate aqueous or non-aqueous organic solvent solution to precipitate cefuroxime sodium crystals. The present invention adopts a one-step method for the recovery and preparation of cefuroxime sodium, without the need to separate and dry cefuroxime acid, thereby reducing the damage to cefuroxime acid, and the water content of the system is low during the recovery and preparation process, which is not suitable for unstable cefuroxime sodium Has a good protective effect.

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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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/34C07D501/04C07D501/12
Inventor 刘丹青冯胜昔姚柳端梁少娟金国有朱艺基王妙英
Owner GUANGZHOU BAIYUNSHAN PHARM CO LTD
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