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Preparation method of moxifloxacin hydrochloride

A technology for moxifloxacin hydrochloride and hydrochloric acid is applied in the field of preparation of moxifloxacin hydrochloride, which can solve the problems of large loss of moxifloxacin hydrochloride, low yield and liquid phase purity, and insufficient product quality, and achieves low total impurity content. , the effect of improving purity and reducing energy consumption

Active Publication Date: 2019-08-20
广西两面针亿康药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the currently disclosed preparation and synthesis methods, the obtained moxifloxacin hydrochloride has relatively large loss, low yield and liquid phase purity, many impurities, and the product quality is not good enough, especially when moxifloxacin hydrochloride is produced industrially.

Method used

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  • Preparation method of moxifloxacin hydrochloride
  • Preparation method of moxifloxacin hydrochloride
  • Preparation method of moxifloxacin hydrochloride

Examples

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Effect test

Embodiment 1

[0035] A preparation method of moxifloxacin hydrochloride, using ethyl 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylate Condensate with (S,S)-2,8-diazabicyclo[4,3,0]nonane as the parent ring, then add 6N hydrochloric acid twice after the alkali hydrolysis is completed, and continuously crystallize two The second time, the crystalline product obtained in the second time was recrystallized once with ethanol to obtain moxifloxacin hydrochloride with high content and high quality. Specific steps are as follows:

[0036] (1) Add the weighed boric acid and zinc chloride into a 50L reaction tank, pump acetic anhydride into the reaction tank, heat with jacket steam under stirring, raise the temperature to 110°C-120°C, and keep the temperature for 2 hours; the heat preservation is over , lower the temperature to below 100°C, pump glacial acetic acid into the reaction tank, raise the temperature to 110°C-120°C, and keep it warm for 1 hour.

[0037] (2) Open ...

Embodiment 2

[0050] A preparation method of moxifloxacin hydrochloride, using ethyl 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylate Condensate with (S,S)-2,8-diazabicyclo[4,3,0]nonane as the parent ring, then add 6N hydrochloric acid twice after the alkali hydrolysis is completed, and continuously crystallize two The second time, the crystalline product obtained in the second time was recrystallized once with ethanol to obtain moxifloxacin hydrochloride with high content and high quality. Specific steps are as follows:

[0051] (1) Add the weighed boric acid and zinc chloride into a 50L reaction tank, pump acetic anhydride into the reaction tank, heat with jacket steam under stirring, raise the temperature to 110°C-120°C, and keep the temperature for 2 hours; the heat preservation is over , lower the temperature to below 100°C, pump glacial acetic acid into the reaction tank, raise the temperature to 110°C-120°C, and keep it warm for 1 hour.

[0052] (2) Ope...

Embodiment 3

[0065] A preparation method of moxifloxacin hydrochloride, using ethyl 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylate Condensate with (S,S)-2,8-diazabicyclo[4,3,0]nonane as the parent ring, then add 6N hydrochloric acid twice after the alkali hydrolysis is completed, and continuously crystallize two The second time, the crystalline product obtained in the second time was recrystallized once with ethanol to obtain moxifloxacin hydrochloride with high content and high quality. Specific steps are as follows:

[0066] (1) Add the weighed boric acid and zinc chloride into a 50L reaction tank, pump acetic anhydride into the reaction tank, heat with jacket steam under stirring, raise the temperature to 110°C-120°C, and keep the temperature for 2 hours; the heat preservation is over , lower the temperature to below 100°C, pump glacial acetic acid into the reaction tank, raise the temperature to 110°C-120°C, and keep it warm for 1 hour.

[0067] (2) Ope...

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Abstract

The invention discloses a preparation method of moxifloxacin hydrochloride. The method comprises the following steps: performing condensation by using 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-ethylquinolinecarboxylate as a central ring, and (S,S)-2,8-diazabicyclo[4,3,0]nonane as a side chain, after alkali hydrolysis is completed, adding a part of 6N hydrochloric acid, performing primary crystallization, adding the remaining 6N hydrochloric acid, performing secondary crystallization, and performing recrystallization on the crystallized product obtain by the secondary crystallization once by using ethanol to obtain the moxifloxacin hydrochloride with a high content and excellent quality. When the method provided by the invention is adopted to prepare the moxifloxacin hydrochloride, product loss caused by repeated crystallization is reduced, labor intensity is reduced, energy consumption is reduced, product stability is improved, product quality is greatly improved, and themethod is suitable for industrialized large-scale production; and the prepared moxifloxacin hydrochloride contains 99.6%-102.0% of C21H25ClFN3O4 calculated by an anhydrate, and has a low total impurity content.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry, in particular to a preparation method of moxifloxacin hydrochloride. Background technique [0002] Moxifloxacin HydrocHloride (Moxifloxacin HydrocHloride) is an ultra-broad-spectrum fluoroquinolone antibacterial drug launched by Bayer Company in Germany. Moxifloxacin Hydrochloride was first listed in Germany in 1999 and is used to treat upper and lower respiratory tract infections (such as: Acute sinusitis, acute exacerbation of chronic bronchitis, community-acquired pneumonia, and skin and soft tissue infections) adults, has strong antibacterial activity, broad antibacterial spectrum, is not easy to produce drug resistance and is effective against common drug-resistant bacteria, long half-life, and less adverse reactions And many other advantages, with the clinical application, its curative effect is more and more affirmed. There are many synthetic methods about moxifloxacin hydroch...

Claims

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Application Information

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IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 莫善军何政剑何群覃旭韦岳正熊春媚韦泰新范桂红黄敏聪赖一竹陆琪锋黄敬洲
Owner 广西两面针亿康药业股份有限公司
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