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Preparation method of Cefazedone sodium salt

A technology of cefoxitone sodium and cefoxime acid, which is applied in the field of medicine, can solve the problems of large pollution, low drying efficiency, and easy residue, and achieve the effects of reducing production costs, shortening the production cycle, and reducing solvent residues

Active Publication Date: 2019-03-29
SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as: in the patent CN101584671, the cefazedone sodium solid is dissolved in water, after decolorization and filtration by activated carbon, acetone is added to the filtrate to crystallize, and the crystals are filtered and dried to obtain cefazedone sodium crystals. The drying method controls moisture, and there are problems such as low drying efficiency and difficulty in reproducing moisture control of different batches of products.
[0007] 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
But the obtained cefazedone sodium fine product is tested, and the moisture is still at 0.9-1.1%.

Method used

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  • Preparation method of Cefazedone sodium salt
  • Preparation method of Cefazedone sodium salt
  • Preparation method of Cefazedone sodium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Add 27.42 g of cefoxime acid to 192 mL of a mixed solvent of methanol and isopropanol (methanol: isopropanol = 1:3 (v / v)), lower the temperature to 8°C, and stir (45HZ) for 5 minutes under temperature control , slowly add methanol / triethylamine (methanol:triethylamine=2:1 (v / v)) mixed solution 23ml, control the addition time for 30min;

[0035] (2) Add 1.35g of activated carbon and stir (45HZ) for 15min, filter and enter the crystallization tank;

[0036] (3) Control the temperature of the reaction solution at 8°C, add acetic acid to adjust the pH value to 5 within 30min, add 1.64g of sodium acetate, after the addition is complete, stir (45HZ) for 30min, cool down to 3°C, add 0.10g of seed crystals, and keep stirring ( 45HZ) 30min;

[0037] (4) Add 3.69g of sodium acetate within 1 hour, keep warm at 3°C ​​to grow crystals for 1.5 hours, add 411.3ml of acetone within 30 minutes, after adding, keep stirring (45HZ) for 2 hours;

[0038] (5) Blowing, vacuum drying, he...

Embodiment 2

[0040] (1) Add 27.42 g of cefoxime acid to 165 ml of a mixed solvent of methanol and isopropanol (methanol: isopropanol = 1:2 (v / v)), lower the temperature to 10°C, and stir under temperature control (45HZ) for 7 minutes , slowly add methanol / triethylamine (methanol:triethylamine=2.5:1 (v / v)) mixed solution 14ml, control the addition time for 20min;

[0041] (2) Add 1.35g of activated carbon and stir (45HZ) for 10min, filter and enter the crystallization tank;

[0042] (3) Control the temperature of the reaction solution at 10°C, add acetic acid to adjust the pH value to 4 within 25min, add 1.23g of sodium acetate, after the addition is complete, stir (45HZ) for 35min, cool down to 3°C, add 0.10g of seed crystals, and keep stirring ( 45HZ) 35min;

[0043] (4) Add 3.28g of sodium acetate within 1h, keep warm at 3°C ​​for 2h, add acetone 274.2ml within 25min, keep stirring (45HZ) for 2.5h;

[0044] (5) Blowing, vacuum drying and heating program: Room temperature rises to 40°C,...

Embodiment 3

[0046] (1) Add 27.42 g of cefoxime acid to 220 ml of a mixed solvent of methanol and isopropanol (methanol: isopropanol = 1:4 (v / v)), cool down to 7°C, stir for 4 minutes under temperature control, and slowly add Methanol / triethylamine (methanol:triethylamine=1.5:1 (v / v)) mixed solution 33ml, control the addition time 40min;

[0047] (2) Add 1.35 g of activated carbon and stir for 20 minutes, filter and enter the crystallization tank;

[0048] (3) Control the temperature of the reaction solution at 7°C, add acetic acid to adjust the pH value to 6 within 35min, add 2.05g of sodium acetate, after the addition is complete, stir (45HZ) for 25min, cool down to 3°C, add 0.10g of seed crystals, and keep stirring ( 45HZ) 25min;

[0049] (4) Add 4.1 g of sodium acetate within 1.5 hours, keep the crystal at 3°C ​​for 1 hour, add 548.4 ml of acetone within 35 minutes, and keep stirring for 1.5 hours;

[0050] (5) Blowing, vacuum drying temperature rise program is room temperature rises t...

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Abstract

The invention provides a preparation method of Cefazedone sodium salt, comprising the following main steps: adding Cefazedone acid into a methanol-isopropanol mixed solvent, adding methanol / triethylamine to carry out a salt forming reaction, regulating pH by adding acetic acid, adding sodium acetate and seed crystals to precipitate out sodium salt, growing the grain, adding acetone to completely precipitate out crystals, carrying out programmable heating and vacuum drying to obtain a finished product. an anhydrous system is adopted in the method without the need of humidification, and moisturecan reach 0.5% and below; the content of residual solvent is low, and the contents of methanol, isopropanol and acetone are all below 0.1%; the production cycle is shortened and the production cost is lowered; and there are few crystal impurities and the purity is high.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of cefazedone sodium. 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. Therefore, there is an urgent need for clinically e...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04C07D501/12
CPCC07D501/04C07D501/12C07D501/36
Inventor 宋丽丽李强孔凡刚
Owner SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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