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A kind of refining method of delafloxacin

A refining method and technology of delafloxacin, applied in the field of medicine, can solve the problems of product residues, single impurity in products that do not meet medicinal requirements, etc.

Active Publication Date: 2018-09-25
YANGTZE RIVER PHARM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese patent applications CN96198104.0, CN200980138280.X, CN201310021838.4, CN201410068991.7 disclose the preparation method of delafloxacin, but the purity of the product obtained by the existing method and the content of individual impurities do not meet the medicinal requirements
[0007] Chinese patent application CN201310124425.9 discloses a method for refining delafloxacin. Although this method can obtain a relatively high-purity product, the solvent used for refining is dioxane, N,N-dimethylformamide, Class II solvents with high boiling point such as N,N-dimethylacetamide, N-methylpyrrolidone, and dimethyl sulfoxide are likely to remain in the product

Method used

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  • A kind of refining method of delafloxacin

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Comparison scheme
Effect test

Embodiment 1

[0042] The preparation of embodiment 1 delafloxacin

[0043] 10g of delafloxacin was dissolved in 170ml of acetone and 80ml of water at 60°C until dissolved. Add 0.1 g of activated carbon, and stir at 60° C. for 20 minutes. Filtrate while hot, cool the filtrate to -10°C and keep stirring for 2 hours for crystallization. After filtration, the filter cake was vacuum-dried at 40° C. to obtain 8.5 g of a light yellow solid, with a yield of 85%, a chromatographic purity of 99.75%, and a maximum of 0.07% impurity.

Embodiment 2

[0044] The preparation of embodiment 2 delafloxacin

[0045] 10g of delafloxacin was dissolved in 500ml of acetone and 50ml of water at 80°C until dissolved. Add 1 g of activated carbon, and stir at 80° C. for 30 minutes. Filtrate while it is hot, cool the filtrate to 20°C and keep stirring and crystallize for 24h. After filtration, the filter cake was vacuum-dried at 60° C. to obtain 8.3 g of a light yellow solid, with a yield of 83%, a chromatographic purity of 99.78%, and a maximum of 0.08% impurity.

Embodiment 3

[0046] The preparation of embodiment 3 delafloxacin

[0047] 10g of delafloxacin was dissolved in 300ml of acetone and 50ml of water at 70°C until dissolved. Add 0.05 g of activated carbon, and stir at 70° C. for 25 minutes. Filtrate while it is hot, cool the filtrate to 0°C and keep stirring and crystallize for 12h. After filtration, the filter cake was vacuum-dried at 50° C. to obtain 8.6 g of a light yellow solid, with a yield of 86%, a chromatographic purity of 99.84%, and a maximum of 0.06% impurity.

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Abstract

{0><}0{>The invention discloses a method for refining delafloxacin. The method comprises the following steps: <0}{0><}0{>(a) dissolving delafloxacin in a mixed solvent of C3-C4 alkyl ketone and water; (b) adding activated carbon for decoloring; (c) filtering, and stirring the filtrate for crystallization; (d) filtering, and drying a filter cake, thereby obtaining high-purity delafloxacin. <0}{0><}0{>The method is good in repeatability, simple and convenient to operate, high in product yield and product purity, and relatively suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for refining delafloxacin. Background technique [0002] The chemical name of Delafloxacin is 1-(6-amino-3,5-difluoro-2-pyridyl)-8-chloro-6-fluoro-7-(3-hydroxy-1-aza -1-cyclobutanyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid, the compound has the following structure: [0003] [0004] Delafloxacin is a fluoroquinolone compound with a new structure (No.: WQ-3034) developed by Japan Yuyong Pharmaceutical Co., Ltd., and then Abbott Company of the United States obtained its development license (No.: ABT-492), and now it is developed by Rib - Company X conducts Phase III clinical trials. [0005] Delafloxacin is a new generation of broad-spectrum fluoroquinolone antibiotics, compared with other quinolone antibacterials, it is more effective against Gram-positive bacteria, especially methicillin-resistant golden yellows that are resistant to other quinolon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/14
CPCC07D401/14
Inventor 袁峰泉陈杨杨赵佳孙晓雷王佩强申新程陈令武
Owner YANGTZE RIVER PHARM GRP CO LTD