Preparation technology of cefotaxime

A preparation process, the technology of cefotaxime, applied in the field of preparation of pharmaceutical compounds, can solve the problems of long production cycle, poor crystal form, prolonging the production cycle, etc., to achieve the expansion of equipment input, shorten the production cycle, and reduce production costs Effect

Inactive Publication Date: 2009-10-21
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The preparation process adopts synthesis, extraction, acidification and crystallization in sequence, the production cycle is long, and there are many types of solvents, difficult recovery, long time for adding acidulant, poor crystal form, and crystal growth process, which further prolongs the production cycle , the product content is low, the quality is unstable, and the yield is very low

Method used

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  • Preparation technology of cefotaxime

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The preparation technology of cefotaxime of the present invention is as follows:

[0018] Synthesis reaction: Add 100ml of dichloromethane to a clean and dry three-necked bottle, cool down to 3 degrees, add 10ml of ethanol, control the temperature below 5 degrees, add 19ml of triethylamine, control the temperature at 8 degrees, add 20g of 7-ACA, 27g of AE-active Ester, react at a controlled temperature of about 15°C until the reaction is clear.

[0019] Acidification and crystallization: add hydrochloric acid to the above reaction solution, adjust the pH value to 2.22, cool down and grow crystals for 60 minutes, filter with suction below 10°C, stir and wash the filter cake once with ethanol, and rinse once. After being pumped dry, it was air-dried to obtain cefotaxime crystalline finished product. The yield of the product is 98.8%, the color is 3Y(-), and other items are in line with the internal control requirements of the enterprise.

Embodiment 2

[0021] The preparation technology of cefotaxime of the present invention is as follows:

[0022] Synthesis reaction: Add 100ml of dichloromethane to a clean and dry three-necked bottle, cool down to 5 degrees, add 17ml of isopropanol, control the temperature below 5 degrees, add 12ml of pyridine, control the temperature at 10 degrees, add 20g of 7-ACA, 27.5g of AE- Active ester, control the temperature to react at about 17°C until the reaction is clear.

[0023] Acidification and crystallization: add a mixture of hydrochloric acid and ethanol to the above reaction solution, adjust the pH value to 2.0, lower the temperature, grow the crystal for 60 minutes, filter with suction below 10°C, and wash the filter cake once with acetone and rinse once. After being pumped dry, it was air-dried to obtain cefotaxime crystalline finished product. The product yield is 99.8%, and the color 3Y(-) and other items all meet the internal control requirements of the enterprise.

Embodiment 3

[0025] The preparation technology of cefotaxime of the present invention is as follows:

[0026] Synthesis reaction: Add 100ml of chloroform to a clean and dry three-necked bottle, cool down to 8 degrees, add 20ml of isopropanol, control the temperature below 5 degrees, add 19ml of triethylamine, control the temperature at 8 degrees, add 20g of 7-ACA, 27.5 gAE-active ester, control the temperature at about 14°C until the reaction is clear.

[0027] Acidification and crystallization: add hydrochloric acid to the above reaction solution, adjust the pH value to 3.0, lower the temperature, grow the crystal for 60 minutes, filter with suction below 10°C, stir and wash the filter cake once with ethanol, and rinse once. After being pumped dry, it was air-dried to obtain cefotaxime crystalline finished product. The product yield is 100.1%, the color is 3Y, and other items are in line with the internal control requirements of the enterprise.

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Abstract

The invention relates to a preparation technology of cefotaxime, belonging to the preparation technology of medical compounds. The technology comprises the following steps: adding 7-ACA and AE-active resin reagents in solvent, and then adding an organic base and an alcohol catalyst to carry out a synthesis reaction. The preparation technology is characterized in that an acidifier is directly added for acidification after the reaction is finished so as to devitrified. The invention has simple and convenient operation, short production period, high product yield and low solvent consumption and can obtain products with uniform crystallized grains, good colors, high purity, low cost and stable quality.

Description

technical field [0001] The invention relates to a preparation process of cefotaxime, which belongs to the preparation technology of pharmaceutical compounds. Background technique [0002] Cefotaxime is the precursor of producing cefotaxime sodium. The original preparation process is extraction after synthesis reaction, layering, taking the liquid layer, adding crystallization solvent and directly acidifying the crystallization. The conventional preparation process is: by 7- ACA reacts with AE-active ester, then adds a crystallization solvent, then adds an acidifying agent for acidification treatment, and precipitates crystals to obtain it. The implementation steps and process reference conditions are as follows: [0003] Synthesis: At 3°C, add solvent, 7-ACA, AE active ester, organic base, alcohol, and protective agent into a clean and dry three-necked bottle and stir rapidly at 3-8°C to make the reaction clear. [0004] Extraction: add water to the above feed liquid three ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/34
Inventor 苗得足王龙科徐金锋曾现华
Owner REYOUNG PHARMA
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