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Method for preparing Sparfloxacin

A technology for weighing sparfloxacin, which is applied in the field of preparation of sparfloxacin, can solve the problems of not being able to meet the use requirements, low purity of sparfloxacin, unreasonable design, etc., and achieve significant economic and social benefits, The effect of good product stability and easy handling

Inactive Publication Date: 2016-10-26
河南精康制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the design of the existing sparfloxacin production and preparation process is not reasonable enough, the production cost is high, the purity of the produced sparfloxacin is low, the production efficiency is low, and it cannot meet the use requirements, and needs to be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A kind of preparation method of sparfloxacin, the preparation method of described sparfloxacin comprises the following production steps: a, condensation reaction: according to the molar ratio of 1:1.5::15, take cis-2,6-di Methylpiperazine, 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, DMF for spare, put into the reaction tank Put in and weigh spare DMF, cis-2,6-dimethylpiperazine and 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo -3-quinoline carboxylic acid, stir, heat up to 110°C, keep warm for reaction, react until the conversion rate of the reaction liquid is greater than 99.0% in HPLC, stop heating, stir and cool down to 30°C; b, discharging and pumping Filtration: discharge the material into the suction filter for suction filtration, carry out solid-liquid separation, and obtain the product solid; c, washing and centrifugation: put the obtained solid into the reaction tank, add 380L of ethanol, stir and wash for 0.5 h...

Embodiment 2

[0019] A kind of preparation method of sparfloxacin, the preparation method of described sparfloxacin comprises the following production steps: a, condensation reaction: according to the molar ratio of 1:1.2::20 take cis-2,6-di Methylpiperazine, 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, and pyridine are reserved for use in the reaction tank Put in and weigh spare pyridine, cis-2,6-dimethylpiperazine and 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo -3-quinoline carboxylic acid, stir, heat up to 110°C, keep warm for reaction, react until the conversion rate of the reaction liquid is greater than 99.0% by HPLC, stop heating, stir and cool down to 20°C; b, discharging and pumping Filtration: discharge the material into the suction filter for suction filtration, carry out solid-liquid separation, and obtain the product solid; c, washing and centrifugation: put the obtained solid into the reaction tank, add 400L of ethanol, stir a...

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Abstract

The invention discloses a method for preparing Sparfloxacin. The method comprises the steps of sequentially adding cis-2,6-dimethylpiperazine, 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinoline carboxylic acid and an aprotic polar solvent into a reaction tank according to a feeding ratio, performing a condensation reaction so as to obtain a wet crude product of Sparfloxacin, carrying out baking on the wet crude product of Sparfloxacin so as to control the water content of the wet crude product of Sparfloxacin, adding the dried Sparfloxacin crude product, an alkaline aqueous solution, water, hydrochloric acid, EDTA and medicinal charcoal into a reaction tank according to a feeding ratio, carrying out heating and stirring, carrying out cooling after dissolving is completed, carrying out discharging, centrifuging and spin-drying so as to obtain a wet Sparfloxacin product, subjecting the wet Sparfloxacin product to drying and performing crushing, thereby obtaining a finished product. As a whole, the method has the advantages that the product is good in stability and easy to treat in medicine processing, and the preparation process is simple.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical production technology, and in particular relates to a preparation method of sparfloxacin. Background technique [0002] Sparfloxacin is a kind of quinolone antibacterial drug, its mechanism of action is to inhibit the DNA gyrase in the process of bacterial DNA synthesis to play a bactericidal effect. It not only has good antibacterial effect on Gram-positive bacteria and Gram-negative bacteria, but also has good antibacterial effect on Mycoplasma, Chlamydia, Legionella, anaerobic bacteria including Bacteroides fragilis and Mycobacterium. Due to its good antibacterial effect, its tablets and capsules have been widely used at home and abroad. [0003] At present, the design of the existing production and preparation process of sparfloxacin is not reasonable enough, the production cost is high, the purity of the produced sparfloxacin is low, the production efficiency is low, it cannot meet th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 李怀生李东倡武玄之伊文峰
Owner 河南精康制药有限公司
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