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Preparation method of cefpiramide sodium

A technology of cefpiramide sodium and cefpiramic acid, which is applied in the direction of organic chemistry, can solve the problems of difficult drying of products, long process time and high residual solvents, and achieve the effects of shortening drying time, high purity and low residual solvents

Active Publication Date: 2019-02-22
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the problems of high residual solvent, a wide variety of solvents, including second-class solvents such as methanol and acetonitrile, difficult drying of the product, long process time, and high production costs.

Method used

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  • Preparation method of cefpiramide sodium
  • Preparation method of cefpiramide sodium
  • Preparation method of cefpiramide sodium

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preparation example Construction

[0030] A preparation method of cefpiramide sodium comprises the steps of preparing cefpiramide salt with cefpiramide as a raw material, forming salt and crystallizing, drying, and purging with atomized water for injection driven by gas before drying.

[0031] The preparation method comprises the following steps:

[0032] A. Add cefpiramin to the solvent Ⅰ which is 3 to 6 times the weight of cefpiramin, and stir at 20 to 30°C to obtain a cefpiramin solution;

[0033] In step A, solvent I is any one or a combination of ethanol, acetone, ethyl acetate, isopropanol or water;

[0034] B. Add an organic base to the cefpiramide solution, stir, and control the pH to be 7.5 to 8.0, then add 5 to 10% of the mass of cefpiramide with activated carbon or white clay, decolorize for 0.5 to 1 hour, and filter to obtain cefpiramide Amine amine salt solution;

[0035] The organic base is any one of diethylamine, triethylamine or isopropylamine;

[0036] C. Add sodium isooctanoate to solvent ...

Embodiment 1

[0043] A preparation method of cefpiramide sodium comprises the steps of preparing cefpiramide salt with cefpiramide as a raw material, forming salt and crystallizing, drying, and purging with atomized water for injection driven by gas before drying.

[0044] The preparation method comprises the following steps:

[0045] A. Add 20kg of cefpiramic acid to the mixed solution of 5L purified water-35L acetone-20L ethyl acetate-60L ethanol, and stir at 20°C to obtain a cefpiramic acid solution;

[0046] B. drip triethylamine in the cefpiramide acid dissolving liquid, stir, control pH to be 7.5, then add 2.0kg gac, stir and decolorize 1h, filter, obtain cefpiramide salt solution;

[0047]C. Add 7.05kg of sodium isooctanoate into 600L of acetone, stir at 30°C, filter to obtain sodium isooctanoate solution, add cefpiramide salt solution to the sodium isooctanoate solution within 30 minutes under stirring, and stir at 10°C Crystal growth 1h;

[0048] D. The crystals are filtered, was...

Embodiment 2～4

[0050] Embodiments 2-4 have the same production process steps as in Embodiment 1, the difference is the selection of process parameters, as shown in Table 1 below.

[0051] Table 1

[0052]

[0053]

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PUM

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Abstract

The invention discloses a preparation method of cefpiramide sodium, belonging to the field of chemical pharmacy. The preparation method comprises the following steps: preparing a cefpiramide amine salt by using a cefpiramide acid as a raw material, carrying out salt formation and crystallization, drying, and driving atomized water for injection by using gas to blow before drying. The preparation method can reduce the solvent residue in the product, is simple, energy-saving and environmentally-friendly and is suitable for large-scale industrial production; and the prepared cefpiramide sodium has the advantages of high purity and good stability.

Description

technical field [0001] The invention relates to a method for refining a compound, in particular to a method for refining a β-lactam antibiotic, and belongs to the field of chemical pharmacy. Background technique [0002] Cefpiramide sodium is a semi-synthetic third-generation cephalosporin with broad antibacterial spectrum and bactericidal activity. It has strong antibacterial activity against Gram-positive bacteria, negative bacteria and anaerobic bacteria, and is quite stable against β-lactamase. . Clinically, it is mainly used for pharyngitis, tonsillitis, acute and chronic bronchitis, pneumonia, pulmonary suppurative disease, pyelonephritis, cystitis, prostatitis, meningitis and gynecological infection caused by sensitive bacterial infection. The chemical name is (6R,7R)-7-[[(2R)-2-(4-hydroxyphenyl)-2-[(6-methyl-4-oxo-1H-pyridine-3-formyl) Amino]acetyl]amino]-3-[(1-methyltetrazol-5-yl)thiomethyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]octane-2 Sodium-ene-2-carboxylate [1-2],...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04C07D501/12
CPCC07D501/04C07D501/12C07D501/36
Inventor 田洪年贾全胡利敏张锁庆李庆伟石春利任峰刘树斌魏宝军贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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