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High-purified cefotiam hydrochloride compound

A technology of cefotiam hydrochloride and cefotiam, which is applied in the field of medicine, can solve problems such as difficult operation, low yield and product purity, and cumbersome reaction steps, and achieve the effects of low cost, improved purity, and optimized product quality

Inactive Publication Date: 2012-01-11
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese patent CN101045700A and Chinese patent CN101096373A all disclose a kind of preparation method of cefotiam hydrochloride, but actual reaction steps are loaded down with trivial details, not easy to operate
[0006] At present, domestically required cefotiam hydrochloride raw materials mainly rely on imports, and some manufacturers also produce them, but the yield and product purity are relatively low. Therefore, a high-purity, high-yield, high-content cefotiam hydrochloride compound become the focus of current research

Method used

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  • High-purified cefotiam hydrochloride compound

Examples

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Effect test

Embodiment 1

[0024] The refining of embodiment 1 cefotiam hydrochloride

[0025] (1) Dissolve 100g cefotiam hydrochloride in 1500ml water, add 2% sodium hydroxide solution to pH 7.2, stir and react for 30 minutes, then add D1300 type macroporous adsorption resin, stir and adsorb at room temperature for 20 minutes, use purification Purify by water elution, collect the eluent, and filter;

[0026] (2) In the filtrate, add dropwise the hydrochloric acid solution of 2mol / L to pH value 5, then add ethanol 1500ml, separate out insoluble matter, stir and react at room temperature for 60 minutes, filter, and dry under reduced pressure at 50°C to obtain 93.0g of cefotiam hydrochloride, The yield was 93.0%, and the HPLC purity was 99.7%.

Embodiment 2

[0027] The refining of embodiment 2 cefotiam hydrochloride

[0028] (1) 100g cefotiam hydrochloride was dissolved in 1500ml water, added 10% sodium bicarbonate solution to a pH value of 8.5, stirred and reacted for 60 minutes, then added BS-55 type macroporous adsorption resin, stirred and adsorbed at room temperature for 30 minutes, Elute and purify with purified water, collect the eluent, and filter;

[0029] (2) Add dropwise 8mol / L hydrochloric acid solution to the pH value of 4 in the filtrate, then add isopropanol 1500ml, precipitate insoluble matter, stir and react at room temperature for 90 minutes, filter, and dry under reduced pressure at 45°C to obtain cefotiam hydrochloride 91.6 g, the yield is 91.6%, and the HPLC purity is 99.6%.

Embodiment 3

[0030] The refining of embodiment 3 cefotiam hydrochloride

[0031] (1) Dissolve 100g cefotiam hydrochloride in 1500ml water, add 5% sodium carbonate solution to a pH value of 7.8, stir and react for 50 minutes, then add D1300 type macroporous adsorption resin, stir and adsorb at room temperature for 30 minutes, use purified water Elution and purification, collecting the eluent, and filtering;

[0032] (2) in the filtrate, dropwise add the hydrochloric acid solution of 4mol / L to pH value 4.5, then add ethanol 1500ml, separate out insoluble matter, stir and react at room temperature for 80 minutes, filter, and dry under reduced pressure at 40°C to obtain cefotiam hydrochloride 92.2g, The yield was 92.2%, and the HPLC purity was 99.7%.

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Abstract

The invention provides a cefotiam hydrochloride compound, which is highly purified and finally obtained by the way of achieving the refine and purification purposes through a specifically designed method of acid-base conversion and macroporous absorption resin adsorption, thus optimizing the quality of preparation products and the safety of clinical medication.

Description

technical field [0001] The invention relates to a cefotiam hydrochloride compound, which can obtain high-purity cefotiam hydrochloride and belongs to the technical field of medicine. Background technique [0002] Cefotiam hydrochloride, chemical name: (6R-trans)-7-[[(2-amino-4-thiazolyl)acetyl]amino]-3-[[[1-[(2-(dimethyl Amino)ethyl]-1H-tetrazol-5-yl]thiomethyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxy Acid dihydrochloride, molecular formula: C 18 h 23 N 9 o 4 S 3 2HCl, molecular weight: 598.6, structural formula: [0003] [0004] Cefotiam hydrochloride is a second-generation cephalosporin antibiotic. Its mechanism of action is to combine with penicillin-binding proteins (PBPs) on the bacterial cell membrane to acylate transpeptidase, inhibit the synthesis of bacterial septum and cell wall, and affect the adhesion of cell wall. The cross-linking of peptide components inhibits cell division and growth, elongates the bacterial form, and finally dissolves ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36C07D501/12
Inventor 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD
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