Preparation method of ceftriaxone sodium

A technology of ceftriaxone sodium and sodium acetate, which is applied in the direction of organic chemistry, can solve the problems of restricting product development prospects, multiple allergies, and high production costs, and achieve the effects of improving overall quality, extraction efficiency, and quality

Inactive Publication Date: 2015-09-02
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this product has encountered two problems in the current production and application: 1. High production cost; 2. There are many allergic phenomena in clinical application
These two points seriously restrict the development prospect of this product at present

Method used

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  • Preparation method of ceftriaxone sodium
  • Preparation method of ceftriaxone sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Add 60ml of dichloromethane, 21ml of methanol, and 3ml of water into a 500ml reaction bottle, and cool down to -5~0°C.

[0031] (2) Add 7-ACT wet powder (approximately 18g in dry form) and 19.1g of AE active ester.

[0032] (3) 60min ~ 120min add 15ml triethylamine.

[0033] (4) Control the temperature at -3-3°C, time the reaction for 2 hours, and start sampling to measure the T salt residue. If the 7-ACT residue is ≤0.1%, it is qualified.

[0034] (5) After the 7-ACT residue is qualified, add (0.5g sodium metabisulfite+30ml water) solution, (7.2g sodium acetate+25ml water) solution, (1.05g sodium hydroxide+ 7ml of water), stirred and reacted for 30-60 minutes. Sodium transfer ends.

[0035] (6) Add an appropriate amount of dichloromethane to the reaction solution, and stir for 5 to 15 minutes to ensure that the phases can be separated.

[0036] (7) Stand still for 10 to 30 minutes, and separate the phases. One aqueous phase and one dichloromethane phase are ob...

Embodiment 2

[0044] (1) Add 60ml of dichloromethane, 21ml of methanol, and 3ml of water into a 500ml reaction bottle, and cool down to -5~0°C.

[0045] (2) Add 7-ACT wet powder (approximately 18g in dry form) and 19.1g of AE active ester.

[0046] (3) 60min ~ 120min add 15ml triethylamine.

[0047] (4) Control the temperature at -3-0°C, time the reaction for 2 hours, and start sampling to measure the T salt residue. If the 7-ACT residue is ≤0.1%, it is qualified.

[0048](5) After the 7-ACT residue is qualified, add (0.5g sodium metabisulfite+30ml water) solution, (7.25g sodium acetate+25ml water) solution, (1.25g sodium hydroxide+ 7ml of water), stirred and reacted for 30-60 minutes. Sodium transfer ends.

[0049] (6) Add an appropriate amount of dichloromethane to the reaction solution, and stir for 5 to 15 minutes to ensure that the phases can be separated.

[0050] (7) Stand still for 10 to 30 minutes, and separate the phases. One aqueous phase and one dichloromethane phase are ob...

Embodiment 3

[0058] (1) Add 60ml of dichloromethane, 21ml of methanol, and 3ml of water into a 500ml reaction bottle, and cool down to -5~0°C.

[0059] (2) Add 7-ACT wet powder (approximately 18g in dry form) and 19.1g of AE active ester.

[0060] (3) 60min ~ 120min add 15ml triethylamine.

[0061] (4) Control the temperature at 0-5°C, time the reaction for 2 hours, and start sampling to measure the T salt residue. If the 7-ACT residue is ≤0.1%, it is qualified.

[0062] (5) After the 7-ACT residue is qualified, add (0.5g sodium metabisulfite+30ml water) solution, (7.2g sodium acetate+25ml water) solution, (1.05g sodium hydroxide+ 7ml of water), stirred and reacted for 30-60 minutes. Sodium transfer ends.

[0063] (6) Add an appropriate amount of dichloromethane to the reaction solution, and stir for 5 to 15 minutes to ensure that the phases can be separated.

[0064] (7) Stand still for 10 to 30 minutes, and separate the phases. One aqueous phase and one dichloromethane phase are obt...

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Abstract

The invention provides a preparation method of ceftriaxone sodium. The preparation method includes steps of (1) cooling dichloromethane, methyl alcohol and water mixed solvent, adding 7-ACT and AE (active ester) and trimethylamine, controlling the temperature and timing to react; (2) sequentially adding sodium hydrogen sulfite, sodium acetate and sodium hydroxide and stirring; adding extractant, stirring, standing and splitting phase; extracting extractant by water and splitting phase, and combining water phase; (3) adding extractant under water-phase stirring, transferring to and filling in a pressure container, removing air bubbles and vibrating hermetically, and taking out after freezing with temperature controlled; (4) removing organic phase, adding activated carbon after solids are melted, stirring to decolorize, and filtering in a decarbonized and aseptic manner; adding filtrate into solvent to crystalize, filtering, washing, drying and packaging. The preparation method is low in technique cost, moderate and safe in reaction conditions, convenient to operate and facilitates industrial production, and the obtained product conforms to quality requirements and has the advantages of few impurities and good crystal forms.

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, also known as ceftriaxone, the original research product name: Rocephine, is a new, long-acting, broad-spectrum third-generation semi-synthetic cephalosporin, belonging to β-lactam antibiotics, by inhibiting the synthesis of bacterial cell walls And play a bactericidal effect. It has strong antibacterial activity against most Gram-positive and negative bacteria. The antibacterial spectrum includes Pseudomonas aeruginosa, Escherichia coli, Klebsiella pneumoniae, Haemophilus influenzae, Enterobacter aerogenes, Proteus, Diococcus and Staphylococcus aureus Wait. Clinically, it is mainly used for meningitis, pneumonia, skin and soft tissue infection, peritonitis, urinary system infection, gonorrhea, liver and gallbladder infection, surgical trauma, sepsis and genital infection of sensitiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/04C07D501/12
CPCC07D501/36C07D501/04C07D501/12
Inventor 胡国刚魏青杰王亚其刘亚林蒋晓声刘树林王瑶
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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