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A kind of cephalosporin compound and preparation method thereof

A technology for cephalosporins and compounds, applied in the field of medicine, can solve the problems of low yield, easy residue, poor fluidity and the like of the preparation method

Active Publication Date: 2018-01-12
SHANDONG LUOXIN PHARMA GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For example, in CN 101584671A, the cefazedone sodium solid is dissolved in water, after activated carbon decolorization and filtration, acetone crystallization is added to the filtrate, and the crystals are filtered and dried to obtain cefazedone sodium crystals. This method is only through conventional drying. There are problems such as low drying efficiency and difficulty in reproducing moisture control in different batches of products.
[0006] CN 102924482A discloses a preparation method of low-water-content cefazedone sodium, which has the following disadvantages: (1) sodium methoxide is used as a salt-forming solvent, and the alkalinity is too strong, so that the cefazedone β-lactam ring is easily destroyed, High impurity content, strong corrosiveness, and large pollution; (2) Isopropanol is used as the crystallization solvent, which has a high boiling point and low volatility, and is easy to remain in the product, increasing the impurity content; (3) The crystallization process uses Seed crystal generation by ultrasonic oscillation seeding method
This preparation method is loaded down with trivial details operation, high to equipment requirement, pollution is big, cost is also high, and the obtained product impurity content is high, and yield is low; (4) preparation method yield is low, only 85%
[0007] CN 104119361A discloses a method for refining an antibiotic compound. First, cefzidone and sodium isooctanoate are placed in anhydrous methanol to form a salt, and then a mixed solvent of acetone and ethyl acetate is used for crystallization and crystal growth, and the obtained cefzidone sodium The high-quality goods have low moisture content, low impurity content, high stability, but poor fluidity
[0008] CN104086571A discloses a preparation method of an anti-infective drug. First, cefozione and sodium sodium acetate are placed in anhydrous methanol to form a salt, and then ethanol and acetone are used for crystallization and crystal growth respectively, and the obtained cefozione sodium fine-quality water Low content, low impurity content, high stability, but poor fluidity

Method used

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  • A kind of cephalosporin compound and preparation method thereof
  • A kind of cephalosporin compound and preparation method thereof
  • A kind of cephalosporin compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: Preparation of cefazedone sodium crystal form compound

[0034] 1) Take 1 kg of crude cefzidone sodium, add it into 15 L of mixed solution A at 30-35° C., stir at a speed of 65 r / min to dissolve all of it, and obtain cefzidone sodium solution; wherein the mixed solution A Prepared for isopropanol and water at a volume ratio of 1:6;

[0035] 2) Naturally cool the cefzidone sodium solution obtained in step 1) to 15-20°C, then add the mixed solvent B at a speed of 15L / min under stirring at a stirring speed of 25r / min, after the addition is completed, cool down to 10°C , maintain the stirring speed, and grow the crystal for 3 hours;

[0036] The mixed solution B is prepared from acetone and water at a volume ratio of 1:3; the volume ratio of the mixed solution B to cefazedone sodium solution is 20:1.

[0037] 3) Cool down to 5°C, continue stirring at a stirring speed for 1 hour; keep the temperature at 0-5°C, let stand for 2 hours to crystallize, filter, was...

Embodiment 2

[0042] Embodiment 2: Preparation of cefazedone sodium crystal form compound

[0043] 1) Take 1 kg of crude cefzidone sodium, add it to 10 L of mixed solution A at 30-35° C., stir at a speed of 55 r / min to dissolve all of it, and obtain cefzidone sodium solution, wherein the mixed solution A Formulated with isopropanol and water at a volume ratio of 1:4;

[0044] 2) Naturally cool down the cefzidone sodium solution obtained in step 1) to 15-20°C, then add the mixed solvent B at a speed of 10L / min under stirring at a stirring speed of 15r / min, after the addition is completed, cool down to 10°C , maintain the stirring speed, and grow the crystal for 2 hours;

[0045] The mixed solution B is prepared from acetone and water at a volume ratio of 1:5; the volume ratio of the mixed solution B to cefazedone sodium solution is 15:1.

[0046] 3) Cool down to 5°C, continue stirring at a stirring speed for 0.5 hours; keep the temperature at 0-5°C, let stand for 4 hours to crystallize, fi...

Embodiment 3

[0050] Embodiment 3: Preparation of cefazedone sodium crystal form compound

[0051] 1) Take 1 kg of crude cefzidone sodium, add it to 13 L of mixed solution A at 30-35° C., stir at a speed of 60 r / min to dissolve all of it, and obtain cefzidone sodium solution; the mixed solution A Prepared for isopropanol and water at a volume ratio of 1:5;

[0052] 2) Naturally cool the cefzidone sodium solution obtained in step 1) to 15-20°C, then add the mixed solvent B at a speed of 12L / min under stirring at a stirring speed of 23r / min, after the addition is completed, cool down to 10°C , maintain the stirring speed, and grow the crystal for 2 hours;

[0053] The mixed solution B is prepared from acetone and water at a volume ratio of 1:4; the volume ratio of the mixed solution B to cefazedone sodium solution is 18:1.

[0054] 3) Cool down to 5°C, continue stirring at a stirring speed for 1 hour; keep the temperature at 0-5°C, let stand for 2 hours to crystallize, filter, wash the filt...

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Abstract

The present invention belongs to the technical field of medicine, and particularly relates to a novel cephalosporin cefazedone sodium crystal form compound and a preparation method thereof. According to the present invention, the cefazedone sodium crystal form compound is a cefazedone sodium hydrate, is different from the cefazedone sodium reported in the prior art, and has the X-ray powder diffraction pattern represented by a Figure 1; and the test results show that the cefazedone sodium hydrate has characteristics of significantly increased stability and good fluidity compared with the cefazedone sodium hydrate in the prior art.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a novel cephalosporin cefazedone sodium crystal form compound and a preparation method thereof. Background technique [0002] Infectious diseases are a common and frequently-occurring disease in clinical practice. According to the report of the World Health Organization (WHO), the number of deaths from infectious diseases is as high as 33.3% of the total number of deaths from various causes. Cephalosporins are the most widely used first-line drugs in clinical practice. In recent years, due to the abuse of antibiotics, many "super bacteria" have emerged, and the problem of bacterial drug resistance has become increasingly serious. The "Administrative Measures for the Clinical Application of Antibacterial Drugs" officially implemented by the state restricts the clinical application of the third-generation and fourth-generation cephalosporins with strong alternatives....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/12C07D501/36
Inventor 李俊广王加成孟凡磊
Owner SHANDONG LUOXIN PHARMA GRP CO LTD
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