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Novel cephalosporin compound and preparation method thereof

A technology of cephalosporins and compounds, applied in the field of medicine, can solve the problems of low yield, high stability and low impurity content of the preparation method

Active Publication Date: 2015-12-16
SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For example, in CN101584671A, the cefazedone sodium solid is dissolved in water, and after activated carbon decolorization and filtration, acetone crystallization is added in the filtrate, and the crystals are filtered and dried to obtain cefazedone sodium crystals. method to control moisture, there are problems such as low drying efficiency and difficulty in reproducing moisture control of different batches of products
[0006] CN102924482A discloses a kind of preparation method of low water content cefazedone sodium, has following shortcoming: (1) adopt sodium methylate as salt-forming solvent, alkalinity is too strong, makes cefazedone β-lactam ring easy to be destroyed, impurity High content, strong corrosiveness, and large pollution; (2) using isopropanol as a crystallization solvent, with a high boiling point and low volatility, which is easy to remain in the product and increase the impurity content; (3) ultrasonic crystallization is used in the crystallization process Oscillatory seeding method produces seeds
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] CN104119361A discloses a method for refining an antibiotic compound. First, cefazedone 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. 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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  • Novel cephalosporin compound and preparation method thereof
  • Novel cephalosporin compound and preparation method thereof
  • Novel cephalosporin compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Preparation of Cefoxidone Sodium Crystalline Compound

[0034] 1) Take 1kg of cefoxidone sodium crude product, add it to 15L of mixed solution A at 30~35°C, and stir at a speed of 65r / min to dissolve all of it to obtain cefoxidone sodium solution; wherein the mixed solution A is It is prepared from isopropanol and water in a volume ratio of 1:6;

[0035] 2) Naturally cooling the cefoxidone sodium solution obtained in step 1) to 15~20°C, then adding mixed solvent B at a speed of 15L / min under stirring at a stirring speed of 25r / min, after adding, cooling to 10°C , keep the stirring speed, and grow the crystal for 3 hours;

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

[0037] 3) Cool to 5°C, keep stirring at a stirring speed for 1 hour; keep the temperature at 0~5°C, stand for 2 hours to crystallize, filter, wash the filter cake with...

Embodiment 2

[0042] Example 2: Preparation of Cefoxidone Sodium Crystal Compound

[0043] 1) Take 1kg of cefoxidone sodium crude product, add it to 10L mixed solution A at 30~35°C, and stir at a speed of 55r / min to make all dissolved, to obtain cefoxidone sodium solution, wherein the mixed solution A is It is prepared from isopropanol and water in a volume ratio of 1:4;

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

[0045] The mixed solution B is prepared by acetone and water in a volume ratio of 1:5; the volume ratio of the mixed solution B and the cefoxidone sodium solution is 15:1.

[0046] 3) Cool to 5°C, keep stirring at a stirring speed for 0.5 hours; keep the temperature at 0~5°C, stand for 4 hours to crystallize, filter, wash the filter cake wi...

Embodiment 3

[0050] Example 3: Preparation of Cefoxidone Sodium Crystalline Compound

[0051] 1) Take 1 kg of cefoxidone sodium crude product, 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 a cefoxidone sodium solution; wherein the mixed solution A is It is prepared from isopropanol and water in a volume ratio of 1:5;

[0052] 2) Naturally cooling the cefoxidone sodium solution obtained in step 1) to 15~20°C, then adding mixed solvent B at a speed of 12L / min under stirring at a stirring speed of 23r / min, after adding, cooling to 10°C , keep the stirring speed, and grow the crystal for 2 hours;

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

[0054] 3) Cool to 5°C, keep stirring at a stirring speed for 1 hour; keep the temperature at 0~5°C, stand for 2 hours to crystallize, filter, wash the filter cake w...

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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 cefoxidone sodium crystal 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 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- and fourth-generation cephalosporins with strong alternatives. Therefore, there i...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/12C07D501/36
Inventor 李俊广王加成孟凡磊
Owner SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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