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A kind of purification method of moxifloxacin hydrochloride and the preparation method of moxifloxacin hydrochloride

A technique for moxifloxacin hydrochloride and a purification method, which is applied in the field of drug synthesis, can solve the problems of low purity, low yield, and large loss of moxifloxacin hydrochloride, and achieve simple purification methods, high purification efficiency, and mild conditions Effect

Active Publication Date: 2021-09-24
WUHAN WUYAO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the purity of the moxifloxacin hydrochloride prepared by this method is relatively low, and the loss in water is relatively large, and the yield is relatively low

Method used

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  • A kind of purification method of moxifloxacin hydrochloride and the preparation method of moxifloxacin hydrochloride
  • A kind of purification method of moxifloxacin hydrochloride and the preparation method of moxifloxacin hydrochloride
  • A kind of purification method of moxifloxacin hydrochloride and the preparation method of moxifloxacin hydrochloride

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Embodiment 1

[0031] The present embodiment provides a kind of purification method of moxifloxacin hydrochloride, it comprises the following steps:

[0032] S1. Add 132L ethanol / water / concentrated hydrochloric acid solution (obtained by mixing 60L ethanol, 60L purified water and 12L concentrated hydrochloric acid) to 15kg crude moxifloxacin hydrochloride, stir and heat up to 90°C to dissolve, and reflux for 30min.

[0033] S2. Filtrate hot, cool the filtrate to 5° C., and stir for 2 hours to carry out crystallization.

[0034] S3. Centrifuge the crystallized solution for 30 min at 2000 rpm to obtain a solid precipitate.

[0035] S4. The above solid precipitate was air-dried at 50° C. for 12 hours to obtain 13.1 kg of light yellow moxifloxacin hydrochloride product with a yield of 87.3%.

Embodiment 2

[0037] The present embodiment provides a kind of purification method of moxifloxacin hydrochloride, it comprises the following steps:

[0038] S1. Add 132L ethanol / water / concentrated hydrochloric acid solution (obtained by mixing 60L ethanol, 60L purified water and 12L concentrated hydrochloric acid) to 15kg of crude moxifloxacin hydrochloride, stir and heat up to 80°C to dissolve, and reflux for 60min.

[0039] S2. Filtrate hot, cool the filtrate to 0°C, and stir for 1 hour to crystallize.

[0040] S3. Centrifuge the crystallized solution at 3000 rpm for 15 min to obtain a solid precipitate.

[0041] S4. The above-mentioned solid precipitate was air-dried at 80° C. for 10 h to obtain 12.8 kg of light yellow moxifloxacin hydrochloride product with a yield of 85.3%.

Embodiment 3

[0043] The present embodiment provides a kind of purification method of moxifloxacin hydrochloride, it comprises the following steps:

[0044] S1. Add 78.65L of ethanol / water / concentrated hydrochloric acid solution (obtained by mixing 13L of ethanol, 65L of purified water and 0.65L of concentrated hydrochloric acid) to 15kg of crude moxifloxacin hydrochloride, stir and heat up to 80°C to dissolve, and reflux for 40min.

[0045] S2. Filtrate hot, cool the filtrate to 10°C, and stir for 2 hours to carry out crystallization.

[0046] S3. Centrifuge the crystallized solution for 30 min at 2000 rpm to obtain a solid precipitate.

[0047] S4. The above solid precipitate was air-dried at 70° C. for 10 h to obtain 12.6 kg of light yellow moxifloxacin hydrochloride product with a yield of 84.0%.

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Abstract

A method for purifying moxifloxacin hydrochloride, which relates to the field of pharmaceutical synthesis, which uses a mixed solvent of ethanol, water and concentrated hydrochloric acid in a specific proportion to dissolve and crystallize crude moxifloxacin hydrochloride, which can obtain high-purity moxifloxacin hydrochloride with high efficiency and high yield. Moxifloxacin hydrochloride products. The purification method is simple and easy, has mild conditions, has the characteristics of high purification efficiency and good purification effect, and is suitable for large-scale industrial production. A method for preparing moxifloxacin hydrochloride, which includes the above-mentioned purification method for moxifloxacin hydrochloride, which can obtain moxifloxacin hydrochloride products with high efficiency and high purity, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a method for purifying moxifloxacin hydrochloride and a method for preparing moxifloxacin hydrochloride. Background technique [0002] Moxifloxacin Hydrochloride (Moxifloxacin Hydrochloride) is the fourth generation of extended-spectrum fluoroquinolone antibacterial drugs, chemical name: 1-cyclopropyl-7-[(S,S)-2,8-diazobicyclo[4.3 .0]nonan-8-yl]-6-fluoro-8-methoxy-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid hydrochloride, the structural formula of which is as follows. [0003] [0004] Moxifloxacin hydrochloride was first developed by Bayer Company of Germany, and was first listed in Germany in September 1999 (trade name Avelox). In December of the same year, it was approved by the US FDA and launched in the US. Infectious diseases in adults caused by susceptible bacteria or strongly suspected to be caused by susceptible bacteria. [0005] There are many synthetic methods for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 田俊锋朱毅朱炎朋杨波郭亚兵
Owner WUHAN WUYAO SCI & TECH
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