Flucloxacillin sodium compound and preparation method thereof

The technology of flucloxacillin sodium and compound is applied in the field of flucloxacillin sodium compound and preparation method thereof, which can solve the problems of low purity of flucloxacillin sodium, and achieve the effects of easy industrial production, high product purity, and improvement of clinical adverse reactions.

Inactive Publication Date: 2012-02-15
HAINAN MEILAN SMITH KLINE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to overcome the defects of the above-mentioned prior art, especially the defect of low purity of fl...

Method used

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  • Flucloxacillin sodium compound and preparation method thereof
  • Flucloxacillin sodium compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Get flucloxacillin sodium crude product 10g (content 89.8%) and dissolve in 100ml water, stir, make it dissolve completely, then add 25ml ether, stir, extract 2 times, liquid separation removes the ether phase that contains impurity, collects water phase.

[0039] Add 20 ml of 1 mol / l sodium methoxide to the water phase, stir at 60°C for 1.5 hours, a solid precipitates, let stand to lower the temperature to room temperature, filter, and collect the filtrate.

[0040] The filtrate was separated and purified with an ICN allumina N neutral alumina chromatographic column with a particle size of 18-32 μm and a pore size of 6 nm, wherein the mobile phase used in the chromatographic column was methanol-water (70:30), and the flow rate was 1.5 ml / min , the column temperature is room temperature, and the detection wavelength is 225nm. Collect the parts of cloxacillin sodium in the eluate, concentrate under reduced pressure at 75° C., and dry in vacuo to obtain 8.8 g of refined fl...

Embodiment 2

[0044] Take flucloxacillin sodium raw material drug (Guilin South Medicine Co., Ltd., batch number H20090054) 10g (content 94.6%), dissolve in 100ml water, stir, make it dissolve completely, then add 50ml ether, stir, extract 3 times, separate liquid The ether phase containing impurities was removed and the aqueous phase was collected.

[0045] Add 20 ml of 1 mol / l potassium methoxide to the water phase, stir at 80°C for 1.5 hours, a solid precipitates, let stand to lower the temperature to room temperature, filter, and collect the filtrate.

[0046] The filtrate was separated and purified with an ICN allumina N neutral alumina chromatographic column with a particle size of 18-32 μm and a pore size of 6 nm, wherein the mobile phase used in the chromatographic column was methanol-water (70:30), and the flow rate was 1.5 ml / min , the column temperature is room temperature, and the detection wavelength is 225nm. Collect the parts of cloxacillin sodium in the eluate, concentrate u...

Embodiment 3

[0051] Take flucloxacillin sodium raw material drug (Zhejiang Jinhua Kangenbei Biopharmaceutical Co., Ltd., batch number H20080051) 10g (content 95.4%), dissolve in 100ml water, stir, make it dissolve completely, then add 30ml ether, stir, extract 3 times , separated to remove the ether phase containing impurities, and collected the water phase.

[0052] Add 20 ml of 1 mol / l potassium methoxide to the water phase, stir at 70°C for 1.5 hours, a solid precipitates, let stand to lower the temperature to room temperature, filter, and collect the filtrate.

[0053] The filtrate is separated and purified with a special neutral alumina chromatographic column for Baker column chromatography with 50-200 μm and a pore size of 6 nm, wherein the mobile phase used in the chromatographic column is methanol-water (70: 30), and the flow rate is 1.5 ml / min. The temperature is room temperature, the detection wavelength is 225nm, and the part of cloxacillin sodium in the eluate is collected, con...

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Abstract

The invention discloses a method for preparing a flucloxacillin sodium compound, which comprises the following steps of: 1, dissolving flucloxacillin sodium serving as a raw material in water, adding a water-immiscible solvent, and extracting to obtain an aqueous phase which is subjected to primary purification and contains the flucloxacillin sodium; 2, adding alkaline metal or alkaline earth metal alkoxide into the aqueous phase for processing, optionally heating during processing, and filtering to obtain filtrate, namely aqueous solution which is subjected to secondary purification and contains the flucloxacillin sodium; and 3, separating and purifying the solution by using a preparative neutral alumina chromatographic column, collecting a flucloxacillin part in eluent, concentrating under reduced pressure, and drying in vacuum to obtain flucloxacillin sodium subjected to tertiary purification. By the method, the quality of a preparation product is improved, and the toxic and side effects of the flucloxacillin sodium in the process of preparing an antibacterial medicine are reduced; and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a flucloxacillin sodium compound and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Flucloxacillin Sodium (Flucloxacillin Sodium), the chemical name is (2S, 5R, 6R)-6-[[3-(2-chloro-6-fluorophenyl)-5-methyl-1,2-oxazole- 4-Formyl]amino]-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid sodium salt, molecular formula C 19 h 16 ClFN 3 NaO 5 S, molecular weight 475.85 structural formula: [0003] [0004] Flucloxacillin sodium is a semi-synthetic penicillin-resistant penicillinase. It is an isoxazole derivative of penicillin. , oxacillin) similar. Mainly by inhibiting the biosynthesis of bacterial cell walls and accelerating the decomposition of bacterial cell walls, thus playing an antibacterial role. Pathogens sensitive to penicillin such as Staphylococcus aureus, Streptococcus pyogenes, Streptococcus viridans, Streptococcus pneumoniae, Liste...

Claims

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Application Information

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IPC IPC(8): C07D499/76C07D499/18A61K31/431A61P31/04
Inventor 杨明贵
Owner HAINAN MEILAN SMITH KLINE PHARMA
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