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Crystallization method of cefixime

A cefixime crystallization technology, which is applied in the preparation of cephalosporins and the crystallization field of cefixime, can solve the problem of unsuitable cefixime capsule subpackage, etc., and achieve the effect of high bulk density and good stability

Inactive Publication Date: 2011-12-07
GUANGZHOU BAIYUNSHAN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the cefixime bulk density prepared by patent document 200910014978.2 is less than 0.5g / ml, which is very unsuitable for subpackaging of cefixime capsules

Method used

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  • Crystallization method of cefixime
  • Crystallization method of cefixime
  • Crystallization method of cefixime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 10 grams of cefixime intermediate A (R is -C (CH 3 ) 3 ) in 100ml of water, cooled to 0-10°C, adding 60ml of 20wt% sodium hydroxide solution and stirring for 10 minutes, adding 36wt% hydrochloric acid to adjust the pH of the solution to 6-7 to obtain cefixime sodium salt solution; Add 1 g of activated carbon to the solution, stir and decolorize for 20 minutes, filter out the activated carbon and wash it with 20ml of water, combine the filtrate and the carbon washing solution to obtain a clear cefixime sodium salt solution; keep the temperature of the solution at 15-20°C, add dropwise 18wt% hydrochloric acid until the pH of the solution is 3.0 to 3.3, stirring to precipitate cefixime crystals, while stirring, monitor the pH of the system with an online pH meter, and maintain the pH of the system by adding 18wt% hydrochloric acid dropwise and controlling the rate of addition of 18wt% hydrochloric acid In the range of 3.0 to 3.3, continue until the pH of the solution is i...

Embodiment 2

[0039] Disperse 10 grams of cefixime (content 94%, yellow in color) in 180ml of water and 50ml of ethanol, cool to 0-10°C, add sodium bicarbonate until the cefixime dissolves (solution pH=6.5-7.5), and then Add 0.5 g of active carbon, stir and decolorize for 20 minutes, filter out active carbon and wash with 20 ml of water, combine the filtrate and the carbon washing liquid to obtain a clear cefixime salt solution; add 30 ml of isopropanol to this solution, and keep the solution temperature at 15 ~25°C, add 10wt% hydrochloric acid dropwise until the pH of the solution is 3.0~3.3, stir to precipitate cefixime crystals, and monitor the pH of the system with an online pH meter while stirring, and use dropwise addition of 10wt% hydrochloric acid and control the dropping speed of 10wt% hydrochloric acid Keep the pH of the solution in the range of 3.0 to 3.3 by means of the method, and continue until the pH of the solution does not fluctuate upwards in the range of 3.0 to 3.3 for 0.5...

Embodiment 3

[0042] 10 grams of cefixime intermediate A (R is -CH 3 ) in 100ml of water, cooled to 0-10°C, adding 60ml of 20wt% sodium hydroxide solution and stirring for 10 minutes, adding 36wt% hydrochloric acid to adjust the pH of the solution to 5.5-6.5 to obtain cefixime sodium salt solution; Add 2 grams of activated carbon to the solution, stir and decolorize for 20 minutes, filter the activated carbon and wash it with 20 ml of water, combine the filtrate and the carbon washing solution to obtain a clear cefixime sodium salt solution; add 4 ml ethyl acetate to the solution, and keep the solution temperature At 25-30°C, add 18wt% hydrochloric acid dropwise until the pH of the solution is 3.3-3.5, stir to precipitate cefixime crystals, and monitor the pH of the system with an online pH meter while stirring, and use dropwise addition of 18wt% hydrochloric acid and control 18wt% Keep the pH of the solution in the range of 3.3 to 3.5 by means of hydrochloric acid drop rate, and continue u...

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Abstract

The invention belongs to the technical field of medicine and relates to a crystallization method of cefixime. The method comprises: adding an acid to a solution of cefixime salt in a mixture of an organic solvent and water or in water at a temperature of 0-40° C., adjusting the pH of the solution to 3.0-3.5 while stirring, and monitoring the system with an online pH meter pH, with the precipitation of cefixime crystals, the pH of the system begins to rise. At this time, by continuously adding acid and controlling the rate of acid addition, the pH of the system has been stabilized in the range of 3.0 to 3.5, so that the cefixime crystals have always been stable. Precipitate in a narrow range of pH=3.0-3.5; when the pH of the system does not fluctuate upward without adding acid dropwise and stabilizes at 3.0-3.5 for at least 30 minutes, stop adding acid, stir, then filter, wash, and dry to obtain cephalosporin Kexime crystals. The cefixime crystals obtained by the method of the invention have high bulk density and good stability, and are especially suitable for making capsule preparations.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a preparation method of cephalosporins, more specifically, to a crystallization method of cefixime. Background technique [0002] Cefixime is the third-generation cephalosporin product developed by Japan's Fujisawa Pharmaceutical Co., Ltd. It was launched in Japan in 1987. Cefixime is a new third-generation high-efficiency broad-spectrum oral cephalosporin antibiotic, which has a broad-spectrum antibacterial effect on Gram-positive and negative bacteria, and is used for the treatment of acute bacterial infectious diseases, upper and lower respiratory tract infections, pneumonia, acute bronchial Acute exacerbation of inflammation and chronic bronchitis, urinary system infection, ear nose throat infection and other diseases. The drug is stable to most β-lactamases, and is the drug with the smallest dosage among all cephalosporin antibiotics used clinically so far, and has a long-la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/22C07D501/04
Inventor 刘丹青冯胜昔梁少娟朱艺基王妙英金国有
Owner GUANGZHOU BAIYUNSHAN PHARM CO LTD
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