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Delafloxacin purifying method

A purification method, a polar aprotic technology, applied in the direction of organic chemistry, etc., can solve the problems such as the inability to reach the medicinal standard, no delafloxacin purification method, etc., and achieve the effect of increasing the preparation cost.

Active Publication Date: 2014-10-15
SHANGHAI INST OF PHARMA IND CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] DelafloXacin and meglumine need to be further refined before salt formation to ensure the purity requirements of its salt medicine, and no matter the delafloxacin prepared by the above-mentioned preparation method becomes meglumine salt, it cannot reach the requirements of pharmaceutical standards
We regret to find that there is no report on the refining method of delafloxacin so far

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation of embodiment 1 compound 1

[0028] According to the method described in Example 70 of patent WO9711068: add 2.00 g of 1-(6-amino-3,5-difluoropyridine- 2-yl)-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid, 1.00 g of 3-hydroxyazetidine hydrochloride and 2.00 g of N-methylpyrrolidine, the resulting mixture was stirred at 85° C. for 10 minutes, and the solvent and the like were distilled off under reduced pressure. Add 10mL of ethanol to the obtained residue, heat to reflux for 10 minutes and let cool, filter the precipitate, wash with ethanol and diisopropyl ether successively to obtain 2.1g of light yellow powder, HPLC purity 95.3%.

Embodiment 2

[0029] The refining of embodiment 2 compound 1

[0030] Add 13g of the crude product of Formula 1 prepared according to Example 1 to 39mL of N,N-dimethylformamide, heat to 100°C and stir to dissolve, slowly add distilled water in batches until it just appears turbid, a total of about 8.5mL, and slowly lower to room temperature , left to cool and crystallize for 8 hours, filtered, the filter cake was washed with ethanol, and spin-dried to obtain 10.9 g of light yellow powder, yield 84%, HPLC purity: 99.5%.

Embodiment 3

[0031] The refining of embodiment 3 compound 1

[0032] Add 13g of the crude intermediate of formula I prepared according to Example 1 to 39mL of dimethyl sulfoxide, heat to 100°C and stir to dissolve, slowly add distilled water in batches until it just appears turbid, a total of about 10.5mL, slowly lower to room temperature, Cool and crystallize for 8 hours, filter, wash the filter cake with ethanol, spin dry to obtain 10.3 g of light yellow powder, yield 79%, HPLC purity: 99.4%.

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Abstract

The invention relates to the technical field of a Delafloxacin purifying method . The Delafloxacin purifying method comprises the following steps: adding Delafloxacin to a polar aprotic solvent, heating, stirring until Delafloxacin is dissolved, adding distilled water, and gradually cooling for crystallizing to obtain highly pure Delafloxacin. Delafloxacin prepared by present synthetic methods needs purification, the preparation using a simple column chromatography mode increases the large scale production difficulty and greatly increases the preparation cost. The method can effectively remove impurities, and makes the compound Delafloxacin have a high purity (above 99.0%) and meet subsequent preparation demands.

Description

technical field [0001] The invention relates to the technical field of a purification method for preparing a novel fluoroquinolone drug-delafloxacin. Background technique [0002] Delafloxacin is a new generation broad-spectrum fluoroquinolone antibiotic. Compared with other quinolone antibacterial agents, this product is more effective against Gram-positive bacteria, especially methicillin-resistant Staphylococcus aureus (MRSA) resistant to other quinolone antibacterial agents. For the first time, the FDA has publicly announced that delafloxacin has been designated as an eligible drug for the treatment of acute bacterial skin and skin structure infections (ABSSSI) and acquired pneumonia (CABP). Its corresponding meglumine salt is shown in the following formula: [0003] [0004] The preparation method of delafloxacin is mainly found in the two patents WO9711068 and WO2006015194 of the original research company Yuyong Pharmaceutical of Japan and Abbott Pharmaceuticals o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/14
CPCC07D401/14
Inventor 孔锐袁哲东刘相奎陈姗
Owner SHANGHAI INST OF PHARMA IND CO LTD
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