Method of preparing cefpirome sulfate

A technology for cefpirome sulfate and cefpirome, which is applied in the direction of organic chemistry and the like, 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 high yield

Inactive Publication Date: 2008-05-07
河北凯盛医药科技有限公司
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  • Summary
  • Abstract
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  • 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 the test sample of cefpirome, add mobile phase and be made into a 0.5mg / ml solution, to obtain final product.

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

[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 cefpirome sulfate. The method comprises the following steps: treating cefpirome hydroiodide salt with basic anion exchange resin in water as a solvent to obtain cefpirome, and then forming a salt with a sufficient amount of sulfuric acid , adding ethanol to precipitate crystals, and obtain cefpirome sulfate. The invention is easy to operate, the obtained product has better quality and higher yield, and avoids the use of highly toxic solvents such as toluene, thereby reducing the pollution of three wastes.

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 Applications(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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