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Preparation process of mezlocillin sodium

A mezlocillin sodium and preparation process technology, applied in the field of compound preparation, can solve the problems of no crystal growth process, low product content, unstable quality, etc., and achieve the effect of easy dissolution, high purity, and stable quality

Active Publication Date: 2007-05-02
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The preparation process uses ethyl acetate as a single solvent, and there is no buffer to directly precipitate crystals, and the addition of sodium salt-forming agent is carried out slowly. There is no crystal growth process, and the crystals are fine and amorphous powder, which is easy to contain impurities. On the low side, the weight content is 86-87%, the quality is not stable, and it is difficult to dissolve

Method used

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  • Preparation process of mezlocillin sodium

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Effect test

Embodiment 1

[0033] The preparation process of mezlocillin sodium according to the present invention is as follows:

[0034] Acylation: At room temperature, add 10g of ampicillin trihydrate and 75ml of water to a clean, dry three-necked flask, and cool to 16°C. After the stirring was turned on, 11.8 kg of 1-chloroformyl-3-methanesulfonyl-2-imidazolidinone was added to the reaction solution in batches, stirred rapidly to make it react, and the pH value was adjusted to 6.8 with sodium bicarbonate. After the addition, the reaction was continued for 20 minutes, and the pH was measured at 6.84.

[0035] Acidification: Add 100ml of ethyl acetate to the above reaction solution, add 1.2M hydrochloric acid dropwise with stirring until the pH of the bottom water liquid is 1.86 and the acidification is completed, separate layers, and take the ester layer. Wash the water layer with 20 ml of ethyl acetate, combine the ethyl acetate solution, add 20 ml of methanol and pass through a microporous filter membr...

Embodiment 2

[0039] The preparation process of mezlocillin sodium according to the present invention is as follows:

[0040] Acylation: At room temperature, add 10g of ampicillin trihydrate and 75ml of water to a clean, dry three-necked flask, and cool to 18°C. After the stirring was turned on, 11.8 kg of 1-chloroformyl-3-methanesulfonyl-2-imidazolidinone was added to the reaction solution in batches, stirred quickly to make it react, and the pH value was adjusted to 6.6 with sodium bicarbonate. After the addition, the reaction was continued for 20 minutes, and the pH was measured to be 6.7.

[0041] Acidification: Add 100ml of ethyl acetate to the above reaction solution, add 1.2M hydrochloric acid dropwise with stirring until the pH of the bottom water is 2, when the acidification is completed, separate the layers, and take the ester layer. Wash the water layer with 20 ml of ethyl acetate, combine the ethyl acetate solution, add 25 ml of methanol and pass through a microporous filter membran...

Embodiment 3

[0046] The preparation process of mezlocillin sodium according to the present invention is as follows:

[0047]Acylation: At room temperature, add 10g of ampicillin trihydrate and 75ml of water to a clean, dry three-necked flask, and cool to 15°C. After the stirring was turned on, 11.8 kg of 1-chloroformyl-3-methanesulfonyl-2-imidazolidinone was added to the reaction solution in batches, stirred quickly to make it react, and the pH value was adjusted to 6.7 with sodium bicarbonate. After the addition, the reaction was continued for 20 minutes, and the pH was measured to be 6.7.

[0048] Acidification: Add 100ml of ethyl acetate to the above reaction solution, add 1.2M hydrochloric acid dropwise with stirring until the pH of the bottom water is 1.9. After the acidification is completed, separate the layers and take the ester layer. Wash the water layer with 20ml ethyl acetate, combine the ethyl acetate solution, add 23ml methanol and pass through a microporous membrane for later us...

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Abstract

Disclosed is a process for preparing mezlocillin sodium belonging to compound preparation technical field. By acylation reaction of aminobenzyl triaqua acid with 1-chloroformyl-3-mesyl-2-imidazolidinone, acidizing after an ethyl acetate solvent being added, esterified layer removing, salifying reaction after a sodium salt forming agent being added, and seedout, the mezlocillin sodium is obtained. In the invention, the mixed solvent is adopted and the speed of adding the sodium salt forming agent is adjusted. There is recrystallization buffer, so the crystal grain is big and the purity is high.

Description

Technical field [0001] The invention relates to a preparation process of mezlocillin sodium and belongs to the technical field of compound preparation. Background technique [0002] Mezlocillin sodium is a new semi-synthetic antibiotic. The existing solvent crystallization process is a single solvent system of ethyl acetate. The specific preparation process is: Ampicillin trihydrate and 1-chloroformyl-3-methylsulfonyl-2 -Imidazolidinone is prepared by acylation reaction, adding ethyl acetate solvent and then acidification treatment, taking the ester layer, adding sodium salt-forming agent for salt-forming reaction, and precipitating crystals. The reference for an implementation process is as follows: [0003] Acylation: Add ampicillin trihydrate and water to a clean, dry three-necked flask at room temperature, and cool to 15-18°C. After turning on the stirring, add 1-chloroformyl-3-methanesulfonyl-2-imidazolidinone (Mezlocillin chloroformyl) to the reaction liquid in batches, sti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D499/76
Inventor 赵玉山苗得足王龙科郑泽生康恒军
Owner REYOUNG PHARMA
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