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Cefoxitin sodium compound and preparation method thereof

A technology for cefoxitin sodium and crystal compounds, which is applied in the field of medicine, can solve the problems of hygroscopicity detection of cefoxitin sodium crystals and the like, and achieves the effects of high purity, simple preparation method and high stability

Inactive Publication Date: 2014-02-26
YOUCARE PHARMA GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Patent applications 201110258682.2, 201210514291.7, and 201310268592.0 disclosed three crystalline compounds of cefoxitin sodium respectively, and disclosed the X-ray powder diffraction patterns of the crystalline compounds respectively. Although they claimed to improve the stability of cefoxitin sodium crystals, they did not The hygroscopicity of the prepared cefoxitin sodium crystals was tested

Method used

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  • Cefoxitin sodium compound and preparation method thereof
  • Cefoxitin sodium compound and preparation method thereof
  • Cefoxitin sodium compound and preparation method thereof

Examples

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Embodiment 1

[0029] Embodiment 1: Preparation of cefoxitin sodium crystalline compound

[0030] 1. Prepare 5 L of saturated aqueous solution of cefoxitin sodium crude product at 65°C;

[0031] 2. Prepare 15L of mixed organic solvent of acetone, ether and acetonitrile; the volume ratio of acetone, ether and acetonitrile in the mixed organic solvent is 3:2:1;

[0032] 3. Cool the organic solvent to 0°C. Under the sound field with a frequency of 25KHz and an output power of 40W, add the saturated aqueous solution of crude cefoxitin sodium to the organic solvent at a constant speed while stirring, and the addition speed is 3 liters / hour; the stirring speed The temperature is 480 rpm; after the addition, continue to stir and cool down, the stirring speed is 240 rpm; stop stirring after cooling down to 0-5 °C, and the cooling rate is 1 °C / hour. Static growth of crystals for 4 hours; after obtaining crystals, filter, wash with absolute ethanol, and vacuum dry for 6 hours to obtain cefoxitin sodi...

Embodiment 2

[0034] Embodiment 2: Preparation of cefoxitin sodium crystal compound

[0035] 1. Prepare 5 L of saturated aqueous solution of cefoxitin sodium crude product at 60°C;

[0036] 2. Prepare 30L mixed organic solvent of acetone, ether and acetonitrile; the volume ratio of acetone, ether and acetonitrile in the mixed organic solvent is 2:1:1;

[0037]3. Cool the organic solvent to 5°C, under a sound field with a frequency of 25KHz and an output power of 80W, add the saturated aqueous solution of crude cefoxitin sodium to the organic solvent at a constant speed while stirring, and the addition speed is 6 liters / hour; the stirring speed The temperature is 480 rpm; after the addition, continue to stir and cool down, the cooling rate is 2°C / hour, and the stirring speed is 120 rpm; stop stirring after cooling down to 1°C; stand for crystal growth for 6 hours; filter after obtaining crystals, Wash with absolute ethanol, and vacuum-dry for 6 hours to obtain cefoxitin sodium crystalline c...

Embodiment 3

[0039] Embodiment 3: Preparation of cefoxitin sodium crystal compound

[0040] 1. Prepare 5 L of saturated aqueous solution of cefoxitin sodium crude product at 68°C;

[0041] 2. Prepare 20L of mixed organic solvent of acetone, ether and acetonitrile, the volume ratio of acetone, ether and acetonitrile in the mixed organic solvent is 3:1:1;

[0042] 3. Cool the organic solvent to 2°C. Under the sound field with a frequency of 25KHz and an output power of 60W, add the saturated aqueous solution of crude cefoxitin sodium to the organic solvent at a constant speed while stirring, and the addition speed is 2 liters / hour; the stirring speed The temperature is 240 rpm; after the addition, continue to stir and cool down, the cooling rate is 2°C / hour; the stirring speed is 120 rpm; stop stirring after cooling down to 1°C; let the crystal grow for 4 hours; filter after obtaining the crystal, Wash with absolute ethanol, and vacuum-dry for 6 hours to obtain cefoxitin sodium crystalline ...

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Abstract

The invention relates to the field of medicines, and particularly relates to a cefoxitin sodium crystal compound and a preparation method thereof. The structural formula of the cefoxitin sodium crystal compound is shown as formula (I). The cefoxitin sodium crystal compound has high purity, is not easy to absorb water, has good stability, and is safe and reliable for clinical application.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a cefoxitin sodium crystal compound and a preparation method thereof. Background technique [0002] Cefoxitin, chemical name (6R,7S-3-carbamoyloxymethyl-7-methoxy-8-oxo-7-2[(2-thienyl)acetamido]-5 -Thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, developed by Merk Company of the United States, and launched in 1994. Cefoxitin is semi-synthesized from methoxycephalosporin C produced by Streptomyces A new class of antibiotics. Cefoxitin binds to one or more penicillin-binding proteins (PBPs), inhibiting the cell wall biosynthesis of cells with active bacterial division, thereby acting as an antibacterial agent. Cefoxitin sodium has an antibacterial effect on influenza in Gram-negative bacteria Sensitive strains of Haemophilus, Klebsiella, Escherichia coli, Morganella morganii, Mirabilis Proteus, Providencia rettgeri and Neisseria gonorrhoeae all had strong antibacterial effects. [000...

Claims

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Application Information

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IPC IPC(8): C07D501/57C07D501/12
CPCC07D501/12C07D501/57
Inventor 李琦杨磊
Owner YOUCARE PHARMA GROUP
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