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, unstable quality, low product content, etc., and achieve the effect of easy dissolution, stable quality and high purity

Active Publication Date: 2005-07-06
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 technology of mezlocillin sodium of the present invention is as follows:

[0034] Acylation: Add 10 g of ampicillin trihydrate and 75 ml of water into a clean and dry three-necked flask at room temperature, and cool down to 16°C. After the stirring was started, 11.8kg of 1-chloroformyl-3-methanesulfonyl-2-imidazolidinone was added to the reaction solution in stages, 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 to be 6.84.

[0035] Acidification: Add 100ml of ethyl acetate to the above reaction solution, add 1.2M hydrochloric acid dropwise under stirring until the pH of the bottom aqueous solution is 1.86, complete the acidification, separate the layers, and take the ester layer. The aqueous layer was washed with 20 ml of ethyl acetate, the ethyl acetate solution was combined, and 20 ml of methanol was added to pass th...

Embodiment 2

[0039] The preparation technology of mezlocillin sodium of the present invention is as follows:

[0040] Acylation: Add 10 g of ampicillin trihydrate and 75 ml of water into a clean and dry three-necked flask at room temperature, and cool down to 18°C. After the stirring was started, 11.8 kg of 1-chloroformyl-3-methanesulfonyl-2-imidazolidinone was added to the reaction solution in stages, stirred rapidly 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 measured pH was 6.7.

[0041] Acidification: Add 100ml of ethyl acetate to the above reaction solution, add 1.2M hydrochloric acid dropwise under stirring until the pH of the bottom aqueous solution is 2, after the acidification is completed, separate the layers, and take the ester layer. The aqueous layer was washed with 20 ml of ethyl acetate, the ethyl acetate solution was combined, and 25 ml of methanol was added to pass t...

Embodiment 3

[0046] The preparation technology of mezlocillin sodium of the present invention is as follows:

[0047]Acylation: Add 10g of ampicillin trihydrate and 75ml of water into a clean and dry three-necked flask at room temperature, and cool down to 15°C. After the stirring was started, 11.8 kg of 1-chloroformyl-3-methanesulfonyl-2-imidazolidinone was added to the reaction solution in stages, stirred rapidly 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 measured pH was 6.7.

[0048] Acidification: Add 100ml of ethyl acetate to the above reaction solution, add 1.2M hydrochloric acid dropwise under stirring until the pH of the bottom aqueous solution is 1.9, after the acidification is completed, separate the layers, and take the ester layer. The aqueous layer was washed with 20 ml of ethyl acetate, combined with the ethyl acetate solution, and 23 ml of methanol was added to pass t...

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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, which 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 subjected to acylation reaction, acidified after adding ethyl acetate solvent, taking the ester layer, adding sodium salt-forming agent to carry out salt-forming reaction, and crystallization is made. An implementation process reference is as follows: [0003] Acylation: At room temperature, add ampicillin trihydrate and water into a clean and dry three-necked bottle, and cool down to 15-18°C. After starting the stirring, add 1-chloroformyl-3-methanesulfonyl-2-imidazolidinone (mezlocillin chloroformyl) to the reaction solution in stag...

Claims

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Application Information

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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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