Preparation method of ceftriaxone sodium

A technology of ceftriaxone sodium and sodium hydroxide, which is applied in the field of preparation of ceftriaxone sodium, can solve the problems that the content of ceftriaxone sodium does not meet the requirements, and achieve the effects of reducing adverse reactions, improving quality, and shortening reaction time

Active Publication Date: 2021-04-20
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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Problems solved by technology

[0007] But the content of the ceftriaxone sodium that above-mentioned patent obtains all falls short of requirement

Method used

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  • Preparation method of ceftriaxone sodium

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[0034] A kind of preparation method of ceftriaxone sodium, is characterized in that: comprise the steps:

[0035] S1. Mix dichloromethane and alcohols in a ratio of 7:1.8 to 2.2 to obtain the first mixed solution, and cool down to -10 to 0°C;

[0036] S2. Mix dichloromethane and AE active ester in a weight ratio of 70:18-20 to obtain a second mixed solution, and cool down to -5-0°C;

[0037] S3. Mix alcohols, water, triethylamine and 7-ACT in a weight ratio of 14:3:6 to 21:18 to obtain a third mixed solution, and lower the temperature to -5 to 0°C;

[0038] S4. Add the third mixed solution, the second mixed solution and triethylamine to the first mixed solution within 90 to 120 minutes simultaneously to obtain the first reaction solution, and control the temperature at -2 to 0°C to continue the reaction until the end point to 7- ACT residue ≤ 2.0%, the added weight of triethylamine is 0.3-1.1 times of 7-ACT;

[0039] S5, add 20mg / ml aqueous sodium hydroxide solution to the f...

Embodiment 1

[0047] A kind of preparation method of ceftriaxone sodium, described preparation method comprises the following steps:

[0048] S1. Mix 10ml of dichloromethane and 4ml of methanol to obtain the first mixed solution, and cool down to -5°C;

[0049] S2, 50ml of dichloromethane and 19.1g of AE active ester are mixed to obtain the second mixed solution, and the temperature is lowered to -1°C;

[0050] S3, 17ml of methanol, 3ml of water, 3-10ml of triethylamine, 18g of 7-ACT were mixed to obtain the third mixed solution, and the temperature was lowered to -1°C;

[0051] S4. Add the third mixed solution, the second mixed solution and 5-12ml triethylamine to the first mixed solution simultaneously within 90-120 minutes to obtain the first reaction solution, and keep it at -2-0°C to continue the reaction until 7- ACT residue ≤ 2.0%;

[0052] S5. Add 70ml of 20mg / ml sodium hydroxide aqueous solution to the first reaction solution at temperature control -2-0°C, then add 0.5g of sodium...

Embodiment 2

[0060] A kind of preparation method of ceftriaxone sodium, described preparation method comprises the following steps:

[0061] S1. Mix 10ml of dichloromethane and 4ml of ethanol to obtain the first mixed solution, and cool down to -5°C;

[0062] S2, 50ml of dichloromethane and 19.1g of AE active ester are mixed to obtain the second mixed solution, and the temperature is lowered to -1°C;

[0063] S3, 17ml of ethanol, 3ml of water, 3-10ml of triethylamine, 18g of 7-ACT were mixed to obtain the third mixed solution, and the temperature was lowered to -1°C;

[0064] S4. Add the third mixed solution, the second mixed solution and 5-12ml triethylamine to the first mixed solution simultaneously within 90-120 minutes to obtain the first reaction solution, and keep it at -2-0°C to continue the reaction until 7- ACT residue ≤ 2.0%;

[0065] S5. Add 70ml of 20mg / ml sodium hydroxide aqueous solution to the first reaction solution at temperature control -2-0°C, then add 0.5g of sodium m...

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Abstract

The invention discloses a preparation method of ceftriaxone sodium, which comprises the following steps: carrying out earlier-stage treatment on AE active ester and 7-ACT to respectively obtain a first mixed solution, a second mixed solution and a third mixed solution, and simultaneously adding the third mixed solution, the second mixed solution and triethylamine into the first mixed solution to obtain a first reaction solution; adding a sodium hydroxide aqueous solution, sodium metabisulfite and EDTA into the first reaction solution, conducting stirring to obtain a second reaction solution, adding dichloromethane into the second reaction solution, conducting standing for phase splitting to obtain a dichloromethane phase and a water phase, adding activated carbon into the water phase for decoloration, conducting vacuum pumping, and then conducting filtering through a decarburization filter to obtain a to-be-crystallized liquid of ceftriaxone acid; treating the ceftriaxone acid to-be-crystallized liquid to obtain a ceftriaxone acid wet product; then obtaining a to-be-crystallized liquid of ceftriaxone sodium; and adding an acetone solution of methanol into the to-be-crystallized liquid of ceftriaxone sodium for crystallization, and conducting filtering, washing and drying to obtain a finished product of ceftriaxone sodium. According to the invention, high-quality ceftriaxone sodium can be obtained.

Description

technical field [0001] The invention relates to a preparation method of ceftriaxone sodium, which belongs to the field of medicinal chemistry. Background technique [0002] Ceftriaxone sodium is a third-generation cephalosporin antibiotic. Strong activity against Enterobacteriaceae bacteria. The MIC90 for Escherichia coli, Klebsiella pneumoniae, Enterobacter aerogenes, Citrobacter freundii, indole-positive Proteus, Prufidenia and Serratia is between 0.12 and 0.25mg / Between L. Enterobacter cloacae, Acinetobacter and Pseudomonas aeruginosa had poor sensitivity to ceftriaxone sodium. It has strong antibacterial effect on Haemophilus influenzae, Neisseria gonorrhoeae and Neisseria meningitidis, and also has good effect on hemolytic streptococcus and pneumococcus. The MIC for Staphylococcus aureus is 2-4mg / L. Methicillin-resistant Staphylococci and Enterococci were resistant to ceftriaxone sodium. Most Bacteroides fragilis are resistant to ceftriaxone sodium. The chemical...

Claims

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Application Information

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IPC IPC(8): C07D501/06C07D501/12C07D501/36
Inventor 胡利敏高燕霞杨梦德吴送姑孙玉双刘萍谷海泽马亚松李敏李世雄张文悦贾金焕
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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