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One-step preparation process of aseptic cefotaxime sodium for injection

A cefotaxime sodium and preparation 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., achieve reduced amount of solvent used, low production cost, and low labor intensity Effect

Active Publication Date: 2006-05-03
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Two-step process operation, poor crystallization, affects product quality, large solvent usage, serious pollution, high labor intensity, long production cycle, large power consumption, high production cost, and low product yield

Method used

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  • One-step preparation process of aseptic cefotaxime sodium for injection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The preparation technology of cefotaxime sodium of the present invention is as follows:

[0025] Add 120ml of toluene and methanol with 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 3 milliliters of concentrated hydrochloric acid, add sodium isooctanoate solution salt forming agent and 0.1 g sodium bisulfite antioxidant at room temperature, react for 10 minutes, then seed and grow crystals for 30 minutes, and then add toluene dropwise 150ml, the temperature of the dropwise addition of toluene is controlled at 20°C, and the drop is completed in 2 hours. After the drop is completed, the crystal is grown for 30 minutes and the material is discharged. The mixture of 50ml ethyl acetate and 5ml absolute ethanol is used to wash the cake, and then add the cake Stir and wash in the mixture of 140ml acetone and 6ml water for 30 m...

Embodiment 2

[0028] Add 120ml 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 it at 7°C for 63 Minutes, add 3ml of concentrated hydrochloric acid after the reaction is clarified, add a salt-forming agent (13 grams of sodium isooctanoate dissolved in a mixture of 15ml of toluene and 15ml of methanol) at room temperature, 0.1g of sodium bisulfite, then add dropwise toluene to slightly When the crystal is cloudy, grow the crystal for 30 minutes, and then add the remaining toluene dropwise. The temperature of the dropwise addition of toluene is controlled at 22°C, a total of 120ml is added, and the drop is completed within 1.5 hours. Wash the cake with a mixture of ester and 5ml of isopropanol, then add the cake to a mixture of 140ml of acetone and 6ml of water, stir and wash for 20 minutes, then discharge the cake, then wash the cake with a small amount of acetone, wet materi...

Embodiment 3

[0030] Add 120ml of toluene and methanol at a volume ratio of 1:0.8 to the three-neck flask to form a mixed solvent, 20ml of triethylamine, cool down to 4°C, add 20g of 7-ACA, 28g of AE-active ester, and keep at 5°C for 65 Minutes, add 1g of trichloromethyl chloroformate after the reaction is clarified, add a salt-forming agent (13 grams of sodium isooctanoate dissolved in 30ml of mixed solvent) at room temperature, 0.1g of sodium bisulfite, add crystal seeds to grow crystals for 30 minutes Minutes, then add the remaining toluene dropwise, the temperature of the dropwise addition of toluene is controlled at 18°C, a total of 120ml is added, and the drop is completed within 1.8 hours. Wash the cake with a mixture of ethanol, then add the cake to a mixture of 150ml acetone and 6ml water, stir and wash for 25 minutes, then discharge the cake, wash the cake with a small amount of acetone, and dry the wet product in vacuum at 50 degrees .

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PUM

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Abstract

The invention relates to a preparation technique for cefotaxime sodium, which comprises: in solvent, reacting between 7-ACA and AE-active ester with amine as intermediate; adding benzothiazole as assisting solvent and sodium salt agent, separating and crystallizing to obtain the product. Wherein, the reaction solvent comprises benzene organic solvent, acetic ester or acetone and alcohol; stirring the 7-ACA and AE-active ester till clear, adding assisting solvent to benzothiazole; degerming, filtering, adding sodium salt agent for reaction; when liquid shows turbid, feeding crystal; separating the crystal by insoluble solvent to cefotaxime sodium, taking crystallization post-treatment and obtaining the product. This invention needs just one-step operation, has good crystallization and short production period, improves product yield, and decreases solvent harm to operation crews.

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. The existing cefotaxime sodium preparation process is divided into two steps. In a single solvent of dichloromethane, 7-ACA and AE-active ester react under the effect of amine intermediate reactant, then add hydrochloric acid to carry out acidification, and then Cool down and decrystallize to obtain cefotaxime; the second step is to dissolve cefotaxime, add a salt-forming agent to carry out a salt-forming reaction, and use acetone to precipitate cryst...

Claims

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Application Information

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IPC IPC(8): C07D501/02C07D501/34
Inventor 赵玉山王龙科康恒军黄文涛
Owner REYOUNG PHARMA
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