Preparation method of high-purity antofloxacin hydrochloride

A technology of sandacin and hydrochloric acid, which is applied in the field of preparation of high-purity Antofloxacin hydrochloride, can solve the problems of high production cost, unreachable purity, waste of raw materials, etc., and achieve the effect of low production cost and less waste of raw materials

Active Publication Date: 2011-06-08
ANHUI GLOBAL PHARM CO LTD
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Problems solved by technology

According to the preparation method disclosed in the CN1055927C patent, the yield of its piper contraction reaction is only 55%, and there is more waste of raw materials and higher production costs, while its purity cannot meet the requirements of the raw material quality standard of antofloxacin hydrochloride

Method used

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  • Preparation method of high-purity antofloxacin hydrochloride

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Embodiment Construction

[0008] The present invention is further illustrated below by way of examples.

[0009] (S)-9,10-difluoro-2,3-dihydro-3-methyl-8-amino-7-oxo-71H-pyrido[1,2,3-de][1,4 ] benzoxazine-6-carboxylic acid (abbreviated as amino levocarboxylate), N-methylpiperazine and pyridine are charged according to the weight ratio of 2.56kg: 4.9kg: 52kg, after stirring and dissolving, the steam is heated to reflux, and the heating temperature React at 115°C±2°C for 10 hours, evaporate pyridine under reduced pressure, put the residue into 10.8kg of ethanol, filter, wash the filter cake with ethanol, and dry under normal pressure or vacuum at 60-100°C for 8 hours to obtain crude Antofloxacin. Put the crude Antofloxacin obtained above and water into an enamel-jacketed reactor at a weight ratio of 2.68kg: 80kg, slowly add hydrochloric acid under stirring to make the pH of the solution 4.0 to 4.5, and keep it for 30 minutes. Filter through a pore filter, put it in a clean reaction kettle, slowly add am...

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Abstract

The invention relates to a preparation method of high-purity antofloxacin hydrochloride, which comprises the preparation of antofloxacin and the preparation of antofloxacin hydrochloride. The preparation reaction yield rate of the antofloxacin is 70-90 percent, and the preparation reaction yield rate of the antofloxacin hydrochloride is 70-80 percent. The preparation method of the high-purity antofloxacin hydrochloride has the advantages of less raw material waste and lower production cost; meanwhile, the purity of the prepared high-purity antofloxacin hydrochloride can reach the requirement of an antofloxacin hydrochloride raw material quality standard.

Description

technical field [0001] The invention relates to a preparation method of high-purity antofloxacin hydrochloride. Background technique [0002] Antofloxacin hydrochloride is an antibacterial drug with the following structural formula: [0003] [0004] Its chemical name is: (S)-9-fluoro-2,3-dihydro-3-methyl-8-amino-10-(4-methyl-1-piperazinyl)-7-oxo-7H - Pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylate hydrochloride, a highly potent anti-infective drug. According to the preparation method disclosed in the CN1055927C patent, the yield of the piperazine reduction reaction is only 55%, and there are many wastes of raw materials and the disadvantages of high production cost. Meanwhile, its purity cannot meet the requirements of the raw material quality standard of antofloxacin hydrochloride. Contents of the invention [0005] The technical problem to be solved by the present invention is to provide a preparation method of high-purity antofloxacin hydrochloride. [0006] In or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D498/06
Inventor 王祥张沭王开孝常世忠魏科
Owner ANHUI GLOBAL PHARM CO LTD
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