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New method for preparing Cefamandole Nafate

A technology of cefamandole sodium and spamandole sodium, which is applied in the field of medicine and can solve the problems of low purity of cefamandole sodium

Inactive Publication Date: 2011-06-15
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In order to overcome the defects of the above-mentioned prior art, especially overcome the low purity of cefamandole sodium prepared by the prior art, the invention provides a method for refining cefamandole sodium compound

Method used

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  • New method for preparing Cefamandole Nafate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Accurately weigh 10 g of cefamandole sodium with a purity of 95% prepared according to US4351947. Add the solution containing cefamandole sodium into the fixed bed filled with D001 type strongly acidic styrene-based cation exchange resin, and continue the exchange until the pH value is adjusted to 3.3. Then, 10% hydrochloric acid aqueous solution was used as eluent for elution, and the eluate was collected and concentrated under reduced pressure. At this time, the purity detected by high performance liquid chromatography was 97.5%.

[0063] Then adjust the pH value to 6.8 with 1M aqueous sodium hydroxide solution when the temperature is raised to 50°C, and filter while hot to remove insoluble matter. At this time, the purity detected by high performance liquid chromatography was 98.4%.

[0064] Raise the temperature to 70°C and keep it for 20 minutes to evaporate the excess water in the cefamandole sodium solution, then add absolute ethanol in batches at a volume rati...

Embodiment 2

[0069] Accurately take by weighing the cefamandole sodium crude drug of 10g purity 97%. Add the solution containing cefamandole sodium into the fixed bed filled with D201 macroporous strongly basic styrene-based anion exchange resin, and continue the exchange until the pH value is adjusted to 2.8. Then 50% sulfuric acid solution was used as eluent for elution, and the eluate was collected and concentrated under reduced pressure. The purity detected by high performance liquid chromatography was 98.5%.

[0070] Then adjust the pH value to 7.5 with 2M aqueous sodium carbonate solution when the temperature is raised to 65°C, and filter while hot to remove insoluble matter. At this time, the purity detected by high performance liquid chromatography was 99.1%.

[0071] Raise the temperature to 80°C and keep it for 30 minutes to evaporate the excess water in the cefamandole sodium solution, then add absolute ethanol in batches at a volume ratio of water to ethanol of 4:6, and slowl...

Embodiment 3

[0076] Accurately take by weighing 10g the crude product cefamandole sodium of purity 96% that makes according to EP0432297. Add the solution containing cefamandole sodium into the reaction tank filled with GB / T 13659-2008 001×7 strongly acidic styrene-based cation exchange resin, and pass CO 2Gas facilitates the exchange until the pH is adjusted to 3.1. Then, 15% hydrochloric acid aqueous solution was used as eluent for elution, and the eluate was collected and concentrated under reduced pressure. At this time, the purity detected by high performance liquid chromatography was 97.9%.

[0077] Then adjust the pH value to 6.6 with 1M sodium acetate aqueous solution when the temperature is raised to 60°C, and filter while hot to remove insoluble matter. At this time, the purity detected by high performance liquid chromatography was 98.8%.

[0078] Raise the temperature to 80°C and keep it for 15 minutes to evaporate the excess water in the cefamandole sodium solution, then add...

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Abstract

The invention relates to a new method for refining Cefamandole Nafate. The method comprises the following steps of: 1), adsorbing the Cefamandole Nafate by using a strongly acidic ion to exchange resin, performing elution, collecting eluent and concentrating under reduced pressure to obtain the Cefamandole Nafate which is primarily purified; 2) neutralizing by using sodium hydroxide aqueous solution or alkaline sodium salt aqueous solution, adjusting the pH value, and filtering under the hot condition to remove undissolved substances so as to obtain the aqueous solution of the Cefamandole Nafate which is secondarily purified; and 3) adding ethanol into the aqueous solution and recrystallizing by controlling the temperature to obtain the Cefamandole Nafate which is tertiarily purified, wherein the volume ratio of the ethanol to the water is 4:6. The Cefamandole Nafate refined products prepared by the method have purity of not less than 99.5 percent and extremely low heavy metal content, wherein the purity of most of the refined products is not less than 99.6 percent.

Description

technical field [0001] The invention relates to a new preparation method of cefamandole sodium, which belongs to the technical field of medicine. Background technique [0002] Cefamandole sodium (Cefamandole Nafate) is a second-generation cephalosporin antibiotic successfully developed by Lilly Company of the United States at first, and its chemical name is 7-D-(2-formyloxyphenylacetamide)-3-[(1 -Methyl-1H-tetrazol-5 base)thiomethyl]-3-cephem-4-sodium carboxylate, the molecular formula is C 19 h 17 N 6 NaO 6 S 2 , the molecular weight is 512.50, and the structural formula is: [0003] [0004] Cefamandole sodium is the prodrug of cefamandole, which is rapidly hydrolyzed into cefamandole in the body, so the antibacterial effects of the two in the body are basically the same. It has a strong effect on Gram-negative bacteria, and has a strong effect on anaerobic Clostridium, meningococcus, Neisseria gonorrhoeae, Escherichia coli, Klebsiella pneumoniae, influenza bacill...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12
CPCA61K31/546C07D501/36C07D501/58A61P31/04
Inventor 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD
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