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Refining process of tosufloxacin tosylate
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A technology of tosufloxacin toluenesulfonate and p-toluenesulfonic acid, which is applied in the field of refining process of tosufloxacin toluenesulfonate, can solve the problems that tosufloxacin toluenesulfonate cannot reach and achieve low cost, The production process is simple and the effect of little pollution
Inactive Publication Date: 2012-07-25
赤峰万泽药业股份有限公司
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Problems solved by technology
Tosufloxacin tosylate produced by the existing technology cannot meet the standards required by overseas customers
Method used
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Embodiment 1
[0014] Embodiment 1: a kind of refining technique of tosufloxacin tosylate, comprises following processing steps:
[0015] (1) Put 12kg of the hydrolyzate of tosufloxacin toluenesulfonate into the reaction kettle, add 240kg of purified water to dissolve, then slowly add 7.3kg of p-toluenesulfonic acid, react at a temperature of 80°C for 1.5 hours, and naturally cool down to room temperature to crystallize ;
[0016] (2) After the crystals are completely precipitated, the filter cake is washed with 80% ethanol solution, and the filter cake is dried to obtain refined tosufloxacin tosylate.
Embodiment 2
[0017] Embodiment 2: a kind of refining process of tosufloxacin tosylate, comprising the following process steps:
[0018] (1) Put 10kg of the hydrolyzate of tosufloxacin toluenesulfonate into the reaction kettle, add 220kg of purified water to dissolve, then slowly add 6.8kg of p-toluenesulfonic acid, react at a temperature of 82°C for 2 hours, and naturally cool down to room temperature to crystallize ;
[0019] (2) After the crystals are completely precipitated, the filter cake is washed with 75% ethanol solution, and the filter cake is dried to obtain refined tosufloxacin tosylate.
Embodiment 3
[0020] Embodiment 3: a kind of refining technique of tosufloxacin tosylate, comprises following processing steps:
[0021] (1) Put 14kg of the hydrolyzate of tosufloxacin toluenesulfonate into the reaction kettle, add 250kg of purified water to dissolve, then slowly add 7.5kg of p-toluenesulfonic acid, react at a temperature of 78°C for 1.8 hours, and naturally cool down to room temperature to crystallize ;
[0022] (2) After the crystals are completely precipitated, the filter cake is washed with 85% ethanol solution, and the filter cake is dried to obtain refined tosufloxacin tosylate.
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Abstract
The invention discloses a refining process of tosufloxacin tosylate, comprising the following steps of: placing hydrolysate of tosufloxacin tosylate into a reaction kettle, dissolving with purified water; then, slowly adding p-toluenesulfonic acid to react for 1-2 hours at the temperature of 75 DEG C to 85 DEG C, cooling naturally to room temperature for crystallizing; and washing a filtering cake with 70 percent-90 percent ethanol solution, and drying the filtering cake to obtain refined tosufloxacin tosylate. The invention has the advantages of simple production process, low cost, high yield and low content of impurities of the tosufloxacin tosylate.
Description
technical field [0001] The invention belongs to the technical field of pharmaceutical and chemical manufacturing, in particular to a process for refining tosufloxacin tosylate. Background technique [0002] Tosufloxacin tosylate, its chemical name is: 7-[3-amino-1-(pyrrolidinyl)]-1-(2,4-difluorophenyl)-6-fluoro-1,4- Dihydro-4-oxo-1,8-naidine-3-carboxylic acid p-toluenesulfonate monohydrate. It is a broad-spectrum antibacterial drug of the quinolone class. It has antibacterial effect on the following bacteria in vitro: Gram-positive bacteria: pneumococcus, streptococcus pyogenes, hemolytic streptococcus, enterococcus, Staphylococcus bacteria, etc. Gram-negative bacteria: Enterobacteriaceae bacteria such as Acinetobacter, Proteus, Citrobacter, Salmonella, Serratia, and Escherichia coli. Other Gram-negative bacteria include Pseudomonas aeruginosa, Neisseria gonorrhoeae, Haemophilus influenzae, etc. Anaerobic bacteria: Peptostreptococcus, Propionibacterium acnes, etc. This ...
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Application Information
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