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Preparation technology of anhydrous crystal of cefotaxime sodium

A technology of cefotaxime sodium and anhydrous crystallization, which is applied in the field of preparation of pharmaceutical compounds, can solve problems such as high moisture content, easy to exceed the moisture standard, and poor stability, and achieve good color, low moisture content and good stability of the product Effect

Inactive Publication Date: 2012-07-18
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the moisture content is high, the stability is poor, and it is easy to exceed the moisture standard stipulated in the 2010 edition of the Chinese Pharmacopoeia.

Method used

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  • Preparation technology of anhydrous crystal of cefotaxime sodium

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Effect test

Embodiment 1

[0019] The preparation technology of described cefotaxime sodium anhydrous crystal comprises the steps:

[0020] (1) Add 90ml of anhydrous methanol and 5.95g of sodium methoxide into the three-necked flask, and dissolve in a water bath at 27.5±2.5°C;

[0021] (2) Add 45.5 g of cefotaxime acid, keep warm at 27.5±2.5°C for 2 hours, and the solution becomes clear;

[0022] (3) Add 1 g of activated carbon and stir for 30 minutes to decolorize;

[0023] (4) Fine filtration, top washing with 20ml of anhydrous methanol;

[0024] (5) In a water bath at 27.5±2.5°C, add 900ml of ethyl acetate dropwise to the filtrate to crystallize;

[0025] (6) Suction filtration after crystal growth for 2 hours, washing with ethyl acetate;

[0026] (7) Control the temperature at 60° C. and vacuum-dry at a vacuum degree of 0.095 MPa to obtain 42.93 g of a solid with a yield of 90% and a moisture content of 0.93%.

Embodiment 2

[0028] The preparation technology of described cefotaxime sodium anhydrous crystal comprises the steps:

[0029] (1) Add 90ml of formamide and 20g of sodium isooctanoate into a three-neck flask, and dissolve in an ice-salt bath at -27.5±2.5°C;

[0030] (2) Add 45.5 g of cefotaxime acid, keep warm at -27.5±2.5°C for 2 hours, and the solution becomes clear;

[0031] (3) Add 1 g of activated carbon and stir for 30 minutes to decolorize;

[0032] (4) Fine filtration, top washing with 20ml of cold formamide;

[0033] (5) Under the condition of ice-salt bath -27.5±2.5°C, add 900ml of acetone dropwise to the filtrate to crystallize;

[0034] (6) Suction filtration after crystal growth for 2 hours, wash material with acetone;

[0035] (7) Vacuum drying at 50° C. and vacuum degree of 0.099 MPa to obtain 42.83 g of solid with a yield of 89.7% and a moisture content of 0.90%.

Embodiment 3

[0037] The preparation technology of described cefotaxime sodium anhydrous crystal comprises the steps:

[0038] (1) Add 90ml of dimethyl sulfoxide and 6g of sodium acetate into a three-necked flask, and dissolve in a water bath at 17.5±2.5°C;

[0039] (2) Add 45.5 g of cefotaxime acid, keep warm at 17.5±2.5°C for 2 hours, and the solution becomes clear;

[0040] (3) Add 1 g of activated carbon and stir for 30 minutes to decolorize;

[0041] (4) Fine filtration, top washing with 20ml dimethyl sulfoxide;

[0042] (5) In a water bath at 17.5±2.5°C, add 900ml of ethyl acetate dropwise to the filtrate to crystallize;

[0043] (6) Suction filtration after crystal growth for 2 hours, washing with ethyl acetate;

[0044] (7) Vacuum drying at 60° C. under temperature control and vacuum degree of 0.097 MPa to obtain 42.83 g of solid, yield of 89.7%, and moisture of 0.72%.

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Abstract

The invention relates to a preparation technology of anhydrous crystals of cefotaxime sodium and belongs to the technical field of preparation of medicine compounds. The preparation technology of anhydrous crystals of cefotaxime sodium is characterized in that under the condition of certain temperature, cefotaxime acid and a salt forming agent are added in anhydrous solvent for the salt forming reaction, and after decolorization and fine filtration, crystallization solvent is dripped for precipitating the crystals. The preparation technology has the advantages of simplicity and convenience in operation, short production period and low energy consumption; the crystals are low in moisture content and good in stability, wherein the moisture content is 0.5% to 1.0%; and the obtained crystals are uniform in crystallized grains, good in color, high in purity and stable in quality.

Description

technical field [0001] The invention relates to a process for preparing anhydrous crystals of cefotaxime sodium, belonging to the technical field of preparation of pharmaceutical compounds. Background technique [0002] The original preparation process of cefotaxime sodium is to carry out a salt-forming reaction between cefotaxime acid and a salt-forming agent in an aqueous solvent, and then add a solvent dropwise to precipitate crystals after decolorization and fine filtration. The disadvantage of this method is that the moisture content is high, the stability is poor, and it is easy to exceed the moisture standard stipulated in the 2010 edition of the Chinese Pharmacopoeia. Contents of the invention [0003] The object of the present invention is to provide a preparation process of cefotaxime sodium anhydrous crystal, the process is easy to operate, short production cycle, low energy consumption, the obtained product has low moisture content, good stability, uniform crys...

Claims

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Application Information

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IPC IPC(8): C07D501/34C07D501/04C07D501/12
Inventor 何茂群苗得足刘元状赵永坤申守刚郭新营
Owner REYOUNG PHARMA
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