Method of preparing cefpirome sulfate

A technology of cefpirome sulfate and cefpirome, which is applied in the direction of organic chemistry, etc., can solve the problems of difficult three-waste treatment and large environmental pollution, and achieves the effects of reducing three-waste pollution, good product quality and simple operation.

Inactive Publication Date: 2011-06-08
河北凯盛医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common feature of these methods is that a large amount of toxic solvent toluene needs to be used in the treatment process, which makes the treatment of the three wastes more difficult and causes great environmental pollution.

Method used

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  • Method of preparing cefpirome sulfate
  • Method of preparing cefpirome sulfate
  • Method of preparing cefpirome sulfate

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0021] Preparation of the test solution Take an appropriate amount of cefpirome test sample, add mobile phase to form a 0.5mg / ml solution, that is, too.

[0022] Preparation of reference substance solution Take an appropriate amount of cefpirome reference substance and add mobile phase to form a 0.005 mg / ml solution.

[0023] Determination method: Take 10 μl of the test solution and the reference solution respectively and inject them into the liquid chromatograph, measure and record the peak area, and calculate the content of the relevant impurities in the test according to the external standard method.

Embodiment 1

[0025] In a 100ml reaction bottle, add 10g of cefpirome hydroiodide, 30ml of pretreated 201×7 type strong basic anion exchange resin and 20ml of deionized water, stir at room temperature until the hydrogen iodide salt is completely dissolved, filter, and the filtrate Add 0.5g of activated carbon to the solution, stir for 30 minutes, filter, cool the aqueous solution to 5°C, adjust the pH to 1.3 with 6N sulfuric acid, then add dropwise cold ethanol, a white precipitate precipitates, keep stirring below 5°C for 2 hours, filter, and use cold ethanol After washing and vacuum drying, 5.5 g of off-white crystals were obtained. Yield 68.8%. Related substances: <2.0%

Embodiment 2

[0027] In a 100ml reaction bottle, add 10g of cefpirome hydroiodide, 40ml of pretreated D262 strong basic anion exchange resin and 30ml of deionized water, stir at room temperature until the hydrogen iodide salt is completely dissolved, filter, and add to the filtrate Activated carbon 0.5g, stirred for 35 minutes, filtered, cooled the aqueous solution to 5°C, adjusted the pH to 1.3 with 6N sulfuric acid, then added dropwise cold ethanol, a white precipitate precipitated, kept stirring below 5°C for 3 hours, filtered, washed with cold ethanol, After vacuum drying, 5.6 g of off-white crystals were obtained. Yield 70.0%. Related substances: <2.0%

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Abstract

The invention discloses a preparation method of sulfuric acid Cefpirome, and has the steps as follows: Cefpirome hydriodate is changed by the resin through using alkaline negative ion and is processed to get the Cefpirome when using water as solvent, thereby forming salt with full sulfuric acid, ethanol is added to separate out crystal, and then sulfuric acid Cefpirome is obtained. The invention has simple operation, and the obtained product has better quality with higher obtaining rate, moreover, and the solvents with bigger toxicity like toluene are avoided from being used, thereby reducingthe three waste pollution.

Description

technical field [0001] The invention relates to a preparation method of cefpirome sulfate, belonging to the field of drug synthesis. technical background [0002] Cefpirome is a fourth-generation cephalosporin with broad-spectrum antibacterial activity and is effective against staphylococci, penicillin-resistant pneumococci and enterococci. The effect on Pseudomonas aeruginosa is similar to that of ceftazidime, and it has a good effect on many antibiotic-resistant pathogenic bacteria. It is the antibiotic with the strongest antibacterial activity against Gram-positive bacteria among the known third-generation and fourth-generation cephalosporins. The sulfate salt of cefpirome is well absorbed in the stomach, so cefpirome is usually prepared in the sulfate form. Its chemical name is: 1-[[7-[[(2-amino-4-thiazolyl)(methoxyimino)acetyl]-amino]-2-carboxy-8-oxo-5-sulfur Hetero-1-azabicyclo[4.2.0]oct-2-en-3-yl]methyl]-6,7-dihydro-5H-cyclopentadienopyridinium sulfate. The structu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/46
Inventor 赵凯侯建平苑洪忠钟南平王景辉马辉苏翠静
Owner 河北凯盛医药科技有限公司
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