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Crystalline azlocillin sodium and preparation thereof

A technology of azlocillin sodium and azlocillin acid, which is applied in organic chemistry and other fields, and can solve problems such as difficult solvent recovery, no practical value, and increased production costs

Inactive Publication Date: 2006-05-31
江西欧氏药业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as the German patent DE 2104580 is in the process of preparing azlocillin acid directly reacts the ethyl acetate solution of azlocillin with the methanol-ether solution of sodium isooctanoate to obtain the sodium salt of azlocillin without separation, but in fact azlocillin The solubility of loxcillin in ethyl acetate is very small, so the method is not of much practical value
In addition, the method adopted by U.S. Patent No. 3,959,258 is to dissolve azlocillin acid in dimethylacetamide, then react with sodium isooctanoate dissolved in ether-methanol mixture, and finally add the reaction solution thus obtained to ether-methanol mixture. The product is precipitated in the mixed solution of methanol. This method also uses a large amount of mixed organic solvent, which makes the recovery of the solvent very difficult and increases the production cost.

Method used

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  • Crystalline azlocillin sodium and preparation thereof
  • Crystalline azlocillin sodium and preparation thereof
  • Crystalline azlocillin sodium and preparation thereof

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preparation example Construction

[0018] In the preparation method of crystalline azlocillin sodium of the present invention, the following are the preferred parameters:

[0019] The reaction temperature is controlled at 0~20℃, especially at 0~10℃; among them, the inorganic base is preferably sodium carbonate, sodium bicarbonate and sodium hydroxide;

[0020] The preferred organic solvents are acetone, ethanol, tetrahydrofuran, or a mixture thereof.

[0021] The crystalline azlocillin sodium prepared by the preferred method not only has a high content, good stability, but also has excellent fluidity, and is suitable for large-scale production of powder injections.

Embodiment 1

[0022] Example 1 Preparation of crystalline azlocillin sodium

[0023] Add 15ml of water and 5g of azlocillin acid to the reaction flask, stir and cool to 0~5℃, add 0.58g of anhydrous sodium carbonate, keep at 0~5℃ for 4 hours, filter, and add 250ml of acetone to the filtrate while stirring , Continue to stir for half an hour and let stand for 4 hours. Filter, wash twice with 30 ml of acetone, drain off, and dry under reduced pressure to obtain 4.2 g of crystalline azlocillin sodium. Purity: 99.13%

[0024] Measured with a DSC differential scanning calorimeter, the measured heat flow curve of azlocillin sodium shows that it has a decomposition point above 224°C.

[0025] 2θ

Embodiment 2

[0026] Example 2 Preparation of crystalline azlocillin sodium

[0027] Add 15ml of water and 5g of azlocillin acid to the reaction flask, stir and cool to 0~5℃, add 0.95g of sodium bicarbonate, keep warm and stir for 5 hours, filter, add 300ml of absolute ethanol under stirring, continue stirring for half an hour, Let it stand for 4 hours, filter, wash twice with 20 ml of absolute ethanol, drain off, and dry under reduced pressure to obtain 3.6 g of crystalline azlocillin sodium. Purity: 98.82%

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Abstract

A crystalline azlocillin sodium and its production are disclosed. It is characterized by displaying the characteristic data described in specifications on differential scanning calorimeter and X-ray powdery diffraction pattern. Its advantages include simple process, low cost, short production period and high purity.

Description

Technical field [0001] The invention relates to crystalline azlocillin sodium and a preparation method thereof. Background technique [0002] Alocillin sodium is a broad-spectrum, highly effective semi-synthetic penicillin. Its chemical name is (2S, 5R, 6R)-3,3-dimethyl-6-[(R)-2-(2-oxo-1-imidazolidinecarboxamido)-2-phenylacetamido ]-7-oxo-4-thia-1-azabicyclo[3,2,0]heptane-2-carboxylate sodium salt. The molecular formula is C 20 H 22 N 5 NaO 6 S, the structural formula is: [0003] [0004] The preparation method of azlocillin sodium is generally to prepare azlocillin sodium solution by reacting azlocillin acid with sodium hydroxide solution, and then obtain the product by freeze-drying. This method often obtains amorphous powders, the product stability is poor, and the production cycle is long, and the cost is also high. In addition, azlocillin sodium can also be prepared by the solvent method. The solvent method refers to the method in which the product is...

Claims

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Application Information

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IPC IPC(8): C07D499/04
Inventor 侯建平赵凯苑洪忠阙日明
Owner 江西欧氏药业有限责任公司
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