Cefodizime sodium compound and novel method thereof

A technology for cefodizime sodium and cefodizime acid, applied in the medical field, can solve problems such as improper production process control, unsatisfactory drug purity and the like, and achieve the effects of low cost, simple and easy process, and high product purity

Inactive Publication Date: 2011-04-13
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Also, in some cases, due to improper control of the production process, the purity of the drug did not meet the requirements

Method used

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  • Cefodizime sodium compound and novel method thereof
  • Cefodizime sodium compound and novel method thereof
  • Cefodizime sodium compound and novel method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] The refining of embodiment 1 cefodizime sodium

[0040] (1) 100g of cefodizime sodium crude product with a purity of 96.7% was dissolved in 1000ml of water, then slowly added dropwise to 0.3mol / L of phosphoric acid, stirred and reacted until the pH of the solution was 2.0, and left to stand for 2h to produce cefodizime acid precipitation , Suction filtration obtains cefodizime acid 88.1g;

[0041] (2) Dissolve 88.1 g of cefodizime acid obtained in the previous step in 260 g of methanol, add 0.52 g of activated carbon, insulate at 50° C. and stir for 20 min, filter for decarburization, and collect the filtrate;

[0042] (3) the filtrate obtained in the previous step is concentrated under reduced pressure, and the preparation chromatographic column is utilized to carry out separation and purification, wherein the mobile phase used in the chromatographic column is a mixed solution of acetonitrile and pH value 9.5 in a volume ratio of 3: 1, The stationary phase filler is s...

Embodiment 2

[0043] The refining of embodiment 2 cefodizime sodium

[0044] (1) the cefodizime sodium crude product that 100g purity is 96.7% is dissolved in 1000ml water, then slowly add the hydrochloric acid of 0.1mol / L, the pH of stirring reaction to solution is 2.5, leaves standstill 1h, produces cefodizime acid precipitation, Suction filtration obtains cefodizime acid 88.9g;

[0045] (2) Dissolve 88.9 g of cefodizime acid obtained in the previous step in 690 g of acetonitrile, add 2.8 g of activated carbon, insulate at 40° C. and stir for 30 min, filter for decarburization, and collect the filtrate;

[0046] (3) The filtrate obtained in the previous step is concentrated under reduced pressure, and the preparation chromatographic column is utilized to carry out separation and purification, wherein the mobile phase used in the chromatographic column is a mixed solution of acetonitrile and pH value 10.5 sodium hydroxide solution with a volume ratio of 3: 1, fixed The phase filler is sel...

Embodiment 3

[0047] The refining of embodiment 3 cefodizime sodium

[0048] (1) the cefodizime sodium crude product that 100g purity is 96.7% is dissolved in 1000ml water, then slowly add the acetic acid of 1.0mol / L, the pH of stirring reaction to solution is 3.0, produces cefodizime acid precipitation, suction filtration obtains cephalosporin Dizinic acid 89.3g;

[0049] (2) Dissolve 89.3g of cefodizime acid obtained in the previous step in 450g of chloroform, add 1.8g of gac, insulate at 50°C and stir for 20min, filter for decarburization, and collect the filtrate;

[0050] (3) the filtrate obtained in the previous step is concentrated under reduced pressure, and the preparation chromatographic column is utilized to carry out separation and purification, wherein the mobile phase used in the chromatographic column is a mixed solution of acetonitrile and pH value 11 in a volume ratio of 3: 1, The stationary phase filler is selected from silica gel, the flow rate is 4.0ml / min, and the colu...

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Abstract

The invention provides a cefodizime sodium compound and a novel method thereof. The purpose of refining purification is achieved by acid-base salifying reaction, activated carbon adsorption and chromatographic column adsorption separation purification, high-purity cefodizime sodium compound is finally obtained, the preparation product quality is improved, the toxic and side effects are reduced, and the safety in the preparation of broad spectrum antibacterial activity medicine usage is ensured; in addition, compared with the prior art, the method is simple, convenient and feasible in process, has low cost, high yield and high product purification, reduces toxic and side effects and is suitable for industrialized production.

Description

technical field [0001] The invention relates to a cefodizime sodium compound and a new method thereof, belonging to the technical field of medicine. Background technique [0002] Cefodizime disodium, the chemical name is (6R, 7R)-7-[(2-amino-4-thiazolyl)-(methoxyimino)acetamido]-3-[[(5-carboxy Disodium methyl-4-methyl-2-thiazolyl)thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate salt, formula C 20 h 18 N 6 Na 2 o 7 S 4 , the structural formula is: [0003] [0004] Cefodizime sodium is the third-generation broad-spectrum semi-synthetic cephalosporin jointly developed by Host Company and Russell Company. It has been listed in Japan, Germany and the United States successively. In addition, there are other third-generation semi-synthetic cephalosporins that do not have immunomodulatory activity. This is related to the unique substituent of cefodizime sodium containing 2-mercapto-4-methyl-5-thiazoleacetic acid (MMTA). Clinically, it is mainly used...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12A61K31/546A61P31/04
Inventor 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD
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