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One-step preparation process of aseptic ceftriaxone sodium for injection

A technology for ceftriaxone sodium and a preparation process, which is applied in the field of compound preparation, can solve the problems of large solvent usage, high production cost, high labor intensity and the like, and achieves less solvent usage, 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, large amount of solvent used, serious pollution, high labor intensity, long production cycle, high production cost and low product yield

Method used

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

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Experimental program
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Effect test

Embodiment 1

[0023] The preparation technology of ceftriaxone sodium of the present invention is as follows:

[0024] Add 50ml of dichloromethane, 20ml of ethanol, 18ml of triethylamine, and 5ml of water into a three-neck flask, stir and cool down under nitrogen protection; at a temperature of 5°C, add 20g of 7-ACT, 20g of AE-active ester, 0.5g of sodium bisulfite Oxygen agent; stirring reaction, temperature 6°C; reaction clarification, adding hydrochloric acid aqueous solution to adjust pH to 3.5, stirring for 30 minutes, adding 10 grams of sodium isooctanoate, layering, filtering; adding acetone insoluble organic solvent dropwise; solution slightly cloudy, adding crystals Seed and grow crystals; add acetone dropwise to crystallize at a temperature of 10°C; suction filter to obtain a crystal filter cake, wash with acetone; dry with hot air at 50°C; dry to obtain the product.

[0025] The dry product was 33.03g, and the yield was 92.78% (based on 7-ACT).

Embodiment 2

[0027] The preparation technology of ceftriaxone sodium of the present invention is as follows:

[0028] Add 50ml of dichloromethane, 20ml of ethanol, 18ml of triethylamine, and 5ml of water into a three-neck flask, stir and cool down under nitrogen protection; at a temperature of 5°C, add 20g of 7-ACT, 20g of AE-active ester, 0.5g of sodium bisulfite Oxygen agent; stirring reaction, temperature 7°C; reaction clarification, adding acetic acid aqueous solution to adjust pH to 4, stirring for 25 minutes, adding 10 grams of sodium acetate, layering, filtering; adding acetone insoluble organic solvent dropwise; the solution is slightly cloudy, add seed crystals Crystal growth; crystallization by adding acetone dropwise at a temperature of 10°C; suction filtering to obtain a crystallization filter cake, washing with acetone; drying with hot air at 50°C; drying to obtain the product.

[0029] The dry product was 33.01g, and the yield was 92.67% (based on 7-ACT).

Embodiment 3

[0031] The preparation technology of ceftriaxone sodium of the present invention is as follows:

[0032] Add 50ml of dichloromethane, 25ml of ethanol, 18ml of triethylamine, and 5ml of water into a three-neck flask, stir and cool down under nitrogen protection; at a temperature of 8°C, add 20g of 7-ACT, 20g of AE-active ester, 0.5g of sodium bisulfite Oxygen agent; stirring reaction, temperature 8°C; reaction clarification, adding hydrochloric acid aqueous solution to adjust PH to 3, stirring for 35 minutes, adding 10 grams of sodium isooctanoate, layering, filtering; adding isopropanol insoluble organic solvent dropwise; the solution is slightly cloudy, Add crystal seeds to grow crystals; add isopropanol dropwise to crystallize at 8°C; suction filter to obtain a crystallization filter cake, wash with isopropanol; dry with hot air at 50°C; dry to obtain the product.

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Abstract

The invention relates to an improved preparation technique for Ceftriaxone Sodium, which comprises: with nitrogen protection, in solvent, reacting between 7-ACT 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 halogenated hydrocarbon of alkane, acetic ester or acetone and alcohol and water; stirring the 7-ACT and AE-active ester till clear, adding assisting solvent of benzothiazole and salt agent; extracting, degerming, filtering, adding insoluble solvent for Ceftriaxone Sodium; when liquid shows turbid, feeding crystal; separating the crystal by insoluble solvent to cefotaxime sodium; cleaning, drying treatment to obtain the product for injection. 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 an improved preparation process of ceftriaxone sodium, which belongs to the technical field of compound preparation. Background technique [0002] Ceftriaxone sodium is the third-generation broad-spectrum cephalosporin, which is widely used in respiratory tract infections and urinary system infections sensitive to this product, including pyelonephritis and gonorrhea, sepsis, meningitis, burn infection, postoperative infection, bone and joint, Soft tissue, skin and wound infection, abdominal infection (peritonitis, bile duct and gastrointestinal tract infection), etc., and infection prevention during surgery. The existing ceftriaxone sodium preparation process is operated in two steps, protected by nitrogen, in a single solvent of dichloromethane, reacted by 7-ACT and AE-active ester under the effect of triethylamine intermediate reactant, adding benzene And thiazole co-solvent, and then add salt-forming agent to obtain crystal...

Claims

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Application Information

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IPC IPC(8): C07D501/02C07D501/36
Inventor 赵玉山苗得足刘伟孙霁红吕含富
Owner REYOUNG PHARMA
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