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Method for synthesizing mezlocillin sodium through solvent method

A technology of mezlocillin sodium and mezlocillin acid, applied in the direction of organic chemistry and the like, achieves the effects of good stability, fast water dissolving speed and high content

Inactive Publication Date: 2010-02-24
SHANDONG RUNZE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these methods have greatly improved the product quality compared with the freeze-drying method, there are still many defects in this synthesis method, especially in product quality and yield, there is still a certain room for improvement.

Method used

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  • Method for synthesizing mezlocillin sodium through solvent method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A salt-forming agent: Dissolve 3.5g of sodium isooctanoate in a mixed solvent of 25ml of isopropyl ether and 5ml of acetone, add 0.1g of activated carbon, stir for 30min to decolorize, and filter through micropores;

[0027] B mezlocillin acid solution: dissolve 10 g of mezlocillin acid in 30 ml of acetone, add 0.3 g of activated carbon, stir for decolorization for 30 min, and filter through micropores;

[0028] C acetone: 10ml microporous filter;

[0029] Slowly add salt-forming agent A and mezlocillin acid solution B into the reaction vessel containing C at the same time at 20°C, control the rate of addition to 0.4ml / min, add about 1 / 3 of the solution, crystallize and grow the crystal for 1 hour, then Carry out the second simultaneous dropwise addition at the same speed, stir and grow the crystal for 2 hours after the drop, cool down at 3°C ​​and filter with suction, wash with 5ml of isopropyl ether, vacuum-0.08Mpa, and vacuum-dry at 40°C for 3h to obtain mezlocillin ...

Embodiment 2

[0032] A salt-forming agent: Dissolve 3.3g of sodium isooctanoate in a mixed solvent of 25ml of isopropyl ether and 10ml of acetone, add 0.1g of activated carbon, stir for 30min to decolorize, and filter through micropores;

[0033] B mezlocillin acid solution: dissolve 10 g of mezlocillin acid in 30 ml of acetone, add 0.3 g of activated carbon, stir for decolorization for 30 min, and filter through micropores;

[0034] C Acetone: 5ml is filtered through microporous;

[0035] Slowly add salt-forming agent A and mezlocillin acid solution B into the reaction container containing C at the same time at 25°C, control the rate of addition to 0.4ml / min, add about 1 / 3 of the solution, crystallize and grow the crystal for 1 hour, then Carry out the second simultaneous dropwise addition at the same speed, stir and grow crystals for 2 hours after dropping, cool down at 5°C and filter with suction, wash with 5ml of isopropyl ether, vacuum-0.09Mpa, and vacuum-dry at 45°C for 4h to obtain m...

Embodiment 3

[0038] A salt-forming agent: Dissolve 3.2g of sodium isooctanoate in a mixed solvent of 20ml of isopropyl ether and 10ml of acetone, add 0.1g of activated carbon, stir for 30min to decolorize, and filter through micropores;

[0039] B mezlocillin acid solution: dissolve 10 g of mezlocillin acid in 30 ml of acetone, add 0.3 g of activated carbon, stir for decolorization for 30 min, and filter through micropores;

[0040] C acetone 5ml and isopropyl ether 5ml mixed solvent are filtered through microporous;

[0041] Slowly add salt-forming agent A and mezlocillin acid solution B into the reaction container containing C at the same time at 25°C, control the rate of addition to 0.4ml / min, add about 1 / 3 of the solution, crystallize and grow the crystal for 1 hour, then Carry out the second simultaneous dropwise addition at the same speed, stir and grow crystals for 2 hours after dropping, cool down at 3°C ​​and filter with suction, wash with 5ml of isopropyl ether, vacuum-0.085Mpa, ...

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Abstract

The invention belongs to the preparation of penicillin pharmaceuticals and particularly relates to a method for synthesizing mezlocillin sodium through solvent method. The preparation method comprisesthe following steps: dissolving mezlocillin in ketone solvent, dissolving sodium isooctanoate in a mixed solvent of ether and ketone, dropwise adding both reactants in a reaction container simultaneously for synthesis, precipitating crystals, filtrating and drying to obtain the finished product. The invention has the advantage of mild reaction, high production yield, good stability, high content,low residual solvent, fast water dissolution rate and the like; in addition, wastewater can not be generated in the production process and the solvent can be recovered for repeated use.

Description

(1) Technical field [0001] The invention belongs to the preparation of penicillins, in particular to a method for synthesizing mezlocillin sodium by a solvent method. (2) Background technology [0002] Mezlocillin sodium is a new type of broad-spectrum semi-synthetic penicillin antibiotics. It is acid-resistant, alkali-resistant, and enzyme-resistant. Antibacterial effect; Clinically, it has good curative effect on bacterial infections such as Pseudomonas aeruginosa, Lebsiella pneumoniae and Streptococcus. [0003] [0004] At present, the production method of mezlocillin sodium is mainly the freeze-drying method, that is, suspending the mezlocillin acid compound in water, adding sodium hydroxide solution to dissolve it, and separating the sodium salt by freeze-drying. This production method cannot be used for salt formation. The product is purified, and the product is an amorphous powder, and the impurities in the reaction process remain in the product, which has the di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/68C07D499/16
Inventor 彭继先朱瑞清孙喜梅马爱花苗国强
Owner SHANDONG RUNZE PHARMA
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