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Method for preparing cefotaxime

A technology of cefotaxime and weak acid, which is applied in the field of preparation of pharmaceutical compounds, can solve problems such as low quality of cefotaxime, difficult production process control, residual tetrahydrofuran solvent, etc., and achieve reliable product quality, increased crystallization yield, The effect of index reduction

Active Publication Date: 2009-12-30
哈药集团股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although such improvement has avoided the problem of a large amount of THF solvent residues, there are still some residues, and the quality level of the prepared cefotaxime is still not high, with an average color grade of 3.5#, turbidity≤3#, and a content of 89%-91%. For this reason, the production control of the next process is relatively difficult, and the export products are required by foreign businessmen not to have tetrahydrofuran solvent residues, the production process control is relatively difficult, and there are occasional problems of exceeding the standard within the product validity period

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In the condensation tank, add 1000L of dichloromethane, at room temperature, add 7-ACA120kg, AE-active ester 160kg, add triethylamine 82.5kg under stirring, control the reaction temperature 20 ℃ ~ 35 ℃, the reaction time is For 40 minutes, after the reaction is completed, extract the condensation liquid with 1000L water, adjust the pH of the water extract to 6.0 with acetic acid, filter the water extract, and then use alumina (model XFA-75150, particle size 150 mesh ≥ 90%, new alumina Before decolorization, it must be activated with 2% acetic acid solution for 12 hours, and then treated with purified water and pH7.0 sodium acetate / acetic acid buffer solution to pH6.0±0.5 for standby) for adsorption decolorization. After treatment, add 500kg of medicinal ethanol to the water extract, add dropwise hydrochloric acid to precipitate crystals, grow crystals for 30 minutes, continue to add hydrochloric acid to adjust the pH to 2.0-3.0, grow crystals for 60 minutes, discharge an...

Embodiment 2

[0036]In the condensation tank, add 1000L of dichloromethane, at room temperature, add 120kg of 7-ACA, 160kg of AE-active ester, add 82.5kg of triethylamine under stirring, control the reaction temperature 20℃~35℃, the reaction time For 40 minutes, after the completion of the reaction, extract the condensate with 1000L water, adjust the pH of the water extract to 5.0 with acetic acid, filter the water extract, and then use aluminum oxide (model XFA-75150, particle size 150 mesh ≥ 90%, freshly oxidized Before the decolorization of aluminum, it should be activated by 2% acetic acid solution for 12 hours, and then treated with purified water and pH7.0 sodium acetate / acetic acid buffer solution to pH6.0±0.5 respectively) for adsorption decolorization. After treatment, add 400kg of medicinal ethanol to the water extract, add hydrochloric acid dropwise to precipitate crystals, grow crystals for 30 minutes, continue to add hydrochloric acid to adjust the pH to 2.0-3.0, grow crystals f...

Embodiment 3

[0039] In the condensation tank, add 1000L of dichloromethane, at room temperature, add 7-ACA120kg, AE-active ester 160kg, add triethylamine 82.5kg under stirring, control the reaction temperature 20 ℃ ~ 35 ℃, the reaction time is For 40 minutes, after the reaction is completed, extract the condensation liquid with 1000L water, adjust the pH of the water extract to 7.0 with acetic acid, filter the water extract, and then use alumina (model XFA-75150, particle size 150 mesh ≥ 90%, new alumina Before decolorization, it must be activated with 2% acetic acid solution for 12 hours, and then treated with purified water and pH7.0 sodium acetate / acetic acid buffer solution to pH6.0±0.5 for standby) for adsorption decolorization. After treatment, add 600kg of medicinal ethanol to the water extract, drop hydrochloric acid to precipitate crystals, grow crystals for 30 minutes, continue to add hydrochloric acid to adjust the pH to 2.0-3.0, grow crystals for 60 minutes, discharge and centri...

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Abstract

The invention relates to a method for preparing cefotaxime, which comprises the following steps: dissolving 7-ACA and AE- active ester in methylene dichloride, adding triethylamine into the solution with stirring and controlling the reaction temperature to be 20 to 35 DEG C and the reaction time to be 30 to 50 minutes; after the reaction is finished, extracting condensed reaction solution with water, adjusting the pH of water extract to 5.0 to 7.0 with weak acid, filtering the water extract, and subjecting the filtered water extract to adsorption bleaching by alumina; and after bleaching, adding ethanol serving as a crystallization dispersant into the water extract, dripping hydrochloric acid to precipitate crystals, growing crystals, centrifuging the solution, washing the crystals with ethanol, and drying the crystals to obtain the cefotaxime.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical compound, in particular to a preparation method of an antibacterial drug cefotaxime. Background technique [0002] The chemical name of cefotaxime is (6R,7R)-3-[(acetoxy)methyl]-7-[(2-amino-4-thiazolyl)-(methoxyimino)acetamido]-8 -Oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, this product is a third-generation cephalosporin, suitable for pneumonia and other diseases caused by sensitive bacteria Respiratory tract infection, urinary tract infection, meningitis, sepsis, abdominal infection, pelvic infection, skin and soft tissue infection, reproductive tract infection, bone and joint infection, etc. [0003] There are two kinds of techniques for the preparation of cefotaxime commonly used at present: [0004] One is to add 450kg of tetrahydrofuran solution into the condensation tank, put 120kg of 7-ACA and 163kg of AE-active ester at room temperature, stir and add 82.3kg of t...

Claims

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Application Information

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IPC IPC(8): C07D501/34C07D501/06C07D501/12
Inventor 谢英新陈玉山崔嵘单力勇徐淑明
Owner 哈药集团股份有限公司
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