Process for preparing cefotaxime sodium

A cefotaxime sodium and a preparation process technology, applied in the field of compound preparation, can solve problems such as large amount of solvent used, poor crystallization condition, affecting product quality, etc., and achieve reduced amount of solvent used, low production cost, and low labor intensity Effect

Inactive Publication Date: 2005-07-06
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Two-step process operation, poor crystallization, affects product quality, large solvent usage, serious polluti...

Method used

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  • Process for preparing cefotaxime sodium

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Effect test

Embodiment 1

[0022] The preparation technology of cefotaxime sodium of the present invention is as follows:

[0023] Add 120ml of toluene and methanol at a volume ratio of 1:1 to form a mixed solvent, 20ml of triethylamine, cool down to 5°C, add 20g of 7-ACA, 28g of AE-active ester, and keep at 5°C for 60 Minutes, after the reaction is clarified, add sodium isooctanoate solution salt forming agent at room temperature, and 0.1g sodium bisulfite antioxidant, then add toluene dropwise to grow crystals for 30 minutes when it is slightly turbid, then add 150ml of toluene dropwise, and then add toluene dropwise The process can be properly cooled to 20°C, and the dripping is completed in 1.5 hours. After the dripping, the crystal is grown for 30 minutes and the material is discharged. The cake is washed with a mixture of 50ml ethyl acetate and 5ml absolute ethanol, and then the cake is added to 140ml acetone and Stir and wash in the mixed solution of 6ml of water for 30 minutes, then discharge th...

Embodiment 2

[0026] Add 130ml of toluene and methanol at a volume ratio of 1:1 to form a mixed solvent, 20ml of triethylamine, cool down to 6°C, add 20g of 7-ACA, 28g of AE-active ester, and keep at 6°C for 65 Minutes, after the reaction is clarified, add salt-forming agent and 0.1g sodium bisulfite antioxidant at room temperature, then add toluene dropwise to grow the crystal for 30 minutes when it is slightly turbid, then add 130ml of toluene dropwise, the temperature can be lowered to 22°C during the dropwise addition of toluene ℃, control the dropping in 2 hours, and feed the crystal for 30 minutes after the dropping, wash the cake with a mixture of 50ml ethyl acetate and 5ml absolute ethanol, and then add the cake to a mixture of 140ml acetone and 6ml water Stir and wash in the liquid for 30 minutes and discharge the material, then wash the material cake with a small amount of acetone, dry the wet product in vacuum at 50° C. for 3 hours, and collect 31.5 grams of dry product cefotaxime...

Embodiment 3

[0029] Add 130ml of toluene and methanol with a volume ratio of 1:1 to form a mixed solvent, 20ml of triethylamine, cool down to 7°C, add 20g of 7-ACA, 28g of AE-active ester, and keep at 8°C for 60 Minutes, after the reaction is clarified, add salt-forming agent and 0.09g sodium bisulfite antioxidant at room temperature, and then add toluene dropwise to grow the crystal for 30 minutes when it is slightly turbid, then add 140ml of toluene dropwise, and the temperature can be lowered to 18% during the dropwise addition of toluene ℃, controlled at 1.7 hours to finish dropping, after dropping, grow the crystal for 30 minutes and discharge the material, wash the cake with a mixture of 50ml ethyl acetate and 5ml methanol, and then add the cake to a mixture of 120ml acetone and 3ml water Stir and wash for 30 minutes and discharge, then wash the cake with a small amount of acetone, dry the wet material under vacuum at 50° C. for 3 hours, and collect 31.7 g of dry product cefotaxime so...

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Abstract

Disclosed is a process for preparing cefotaxime sodium belonging to compound preparation technical field. In a solvent, 7-ACA reacts with AE-active ester under the action of amine intermediate reactant, then a sodium salt forming agent is added in, and the cefotaxime sodium is obtained after reaction and seedout. The invention is characterized in that the solvent is a mixed solvent composed of benzene organic solvent, ethyl acetate, or acetone and alcohol organic solvent. The technological process is simplified, and the product yield is high.

Description

technical field [0001] The invention relates to a preparation process of cefotaxime sodium, which belongs to the technical field of compound preparation. Background technique [0002] Cefotaxime sodium is a third-generation cephalosporin derivative, widely used in the treatment of sepsis, suppurative meningitis and respiratory tract, urinary tract, biliary tract, bone and joint, skin and soft tissue, abdominal cavity and digestive tract caused by sensitive bacteria. , facial features, genitals and other parts of the infection. Existing cefotaxime sodium preparation process is operated in two steps, in dichloromethane single solvent, by 7-ACA and AE-active ester react under the effect of amine intermediate reactant (being condensing agent), then add Acidify with hydrochloric acid, then cool down and crystallize to obtain cefotaxime; in the second step, dissolve cefotaxime, add a salt-forming agent to carry out a salt-forming reaction, and use acetone to precipitate crystals....

Claims

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Application Information

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IPC IPC(8): C07D501/34
Inventor 赵玉山王龙科康恒军黄文涛
Owner REYOUNG PHARMA
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