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Preparation method of ceftazidime pentahydrate

A technology for ceftazidime and ceftazidime dihydrochloride, applied in the field of chemical pharmacy, can solve the problems of high impurity content of ceftazidime and large crystals, and achieve the effects of low impurity content, simple preparation method and high stability

Active Publication Date: 2019-05-31
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method only adopts one crystallization, the crystal is larger, and the ceftazidime impurity content obtained is higher

Method used

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  • Preparation method of ceftazidime pentahydrate
  • Preparation method of ceftazidime pentahydrate
  • Preparation method of ceftazidime pentahydrate

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preparation example Construction

[0026] A preparation method of ceftazime comprises the step of crystallizing ceftazime dihydrochloride as a raw material, and the crystallization is tertiary crystallization. The pH is adjusted to 2.8-2.9 during the first crystallization, the pH is adjusted to 3.4-3.6 during the second crystallization, and the pH is adjusted to 3.8-3.9 during the third crystallization.

[0027] The preparation method comprises the following steps:

[0028] A. Add ceftazidime dihydrochloride to purified water, stir at 0-10°C, add activated carbon or white clay, decolorize for 0.5-1 hour, filter to obtain ceftazime dihydrochloride decolorization solution;

[0029] The ratio of the volume of purified water in milliliters to the mass of ceftazidime dihydrochloride in grams is 5-6:1, and the amount of decolorizing agent added is 0.5-1% of the mass of ceftazidime dihydrochloride;

[0030] B. Add acetone or ethanol to the decolorization solution of ceftazidime dihydrochloride, add 3-5 mol / L sodium h...

Embodiment 1

[0036] A preparation method of ceftazime comprises the step of crystallizing ceftazime dihydrochloride as a raw material, and the crystallization is tertiary crystallization.

[0037] The preparation method comprises the following steps:

[0038] A. Add ceftazidime dihydrochloride to purified water, stir at 0°C, add activated carbon, decolorize for 0.5h, filter to obtain ceftazidime dihydrochloride decolorization solution;

[0039] The ratio of the volume milliliters of purified water to the mass grams of ceftazime dihydrochloride is 5:1, and the amount of decolorizer is 0.5% of the mass of ceftazidime dihydrochloride;

[0040] B. Add acetone to the ceftazime dihydrochloride decolorization solution, add 3mol / L sodium hydroxide solution to adjust the pH to 2.8, add 1‰ of ceftazime dihydrochloride seed crystals, and grow crystals at a temperature of 8°C , the crystal growth time is 2h;

[0041] The volume milliliters of acetone or ethanol and the mass gram ratio of ceftazidime...

Embodiment 2～4

[0046] Embodiments 2-4 have the same production process steps as in Embodiment 1, the difference is the selection of process parameters, as shown in Table 1 below.

[0047] Table 1

[0048]

[0049]

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Abstract

The invention discloses a preparation method of ceftazidime pentahydrate and belongs to the field of chemical pharmacy. The preparation method includes that ceftazidime dihydrochloride is taken as a raw material for three times crystallization. With the method, the use of acid solutions and alkali solutions can be reduced, and the obtained ceftazidime dihydrochloride has the advantages of low impurity content, high stability and good solubility; the method is simple in preparation, energy-saving and environment friendly and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for preparing a β-lactam antibiotic, and belongs to the field of chemical pharmacy. Background technique [0002] Ceftazidime is a third-generation cephalosporin antibiotic, which has a strong effect on Gram-positive or negative bacteria. It is effective against Pseudomonas aeruginosa, E. Neisseria gonorrhoeae, Neisseria meningitidis, Staphylococcus aureus, hemolytic streptococcus, pneumococcus and bacillus aerogenes have strong antibacterial activity, especially for Pseudomonas aeruginosa, ceftazidime is the most effective antibiotic, its drug The injection is a sterile mixture of ceftazidime pentahydrate and sodium carbonate or arginine. The chemical name is (6R,7R)-7-[[(2Z)-2-(2-amino-1,3-thiazol-4-yl)-2-(1-hydroxy-2-methyl-1-oxy Propan-2-yl)oxyiminoacetyl]amino]-8-oxo-3-(pyridin-1-ium-1-ylmethyl)-5-thia-1-azabicyclo[4.2.0 ] Oct-2-ene-2-carboxylic acid pentahydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/46C07D501/12
Inventor 田洪年贾全胡利敏张锁庆李庆伟石春利任峰刘树斌魏宝军贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA