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Preparation method, detecting method and application of moxifloxacin hydrochloride impurity

A technology for moxifloxacin hydrochloride and impurities, which is applied in the field of medicinal chemistry, can solve problems such as operation danger, and achieve the effects of good control and simple preparation method.

Active Publication Date: 2015-01-21
NANJING CHIA TAI TIANQING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The preparation method uses dangerous sodium azide to replace fluorine. Sodium azide is a highly flammable and explosive drug, and the operation is dangerous.

Method used

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  • Preparation method, detecting method and application of moxifloxacin hydrochloride impurity
  • Preparation method, detecting method and application of moxifloxacin hydrochloride impurity
  • Preparation method, detecting method and application of moxifloxacin hydrochloride impurity

Examples

Experimental program
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Effect test

Embodiment 1

[0052] 1-Cyclopropyl-7-(2,4-dimethoxybenzylamino)-6-fluoro-8-methoxy-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid ethyl ester preparation of

[0053] Add 100g of ethyl 1-cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxo-3-quinolinecarboxylate into the three-necked flask, and then add 600mL of DMF to it: DMSO=1:1 mixed solvent, stir, add 54mL of 2,4-dimethoxybenzylamine, raise the temperature to 120°C for 6h, cool down, pour the reaction solution into 1mol / L dilute hydrochloric acid, stir, add 500mLEA to extract , the organic layer was separated, and the aqueous phase was extracted with EA 300mL×2. The organic layers were combined, dried, filtered and evaporated to dryness to obtain 92.3g of a yellow product, which was directly used in the next step without purification.

Embodiment 2

[0055] 1-Cyclopropyl-7-(2,4-dimethoxybenzylamino)-6-fluoro-8-methoxy-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid ethyl ester preparation of

[0056]Add 100g of ethyl 1-cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxo-3-quinolinecarboxylate into the three-necked flask, then add 600mL of acetone to it, Stir, add 45mL of p-methoxybenzylamine, raise the temperature to 120°C for 6h, cool down, pour the reaction solution into 1mol / L dilute hydrochloric acid, stir, add 500mLEA for extraction, separate the organic layer, and add 300mL×2 EA to the water phase Extract, combine the organic layers, dry, filter and evaporate to dryness to obtain 92.3 g of yellow product, which is directly used in the next step without purification.

Embodiment 3

[0058] 1-Cyclopropyl-7-(2,4-dimethoxybenzylamino)-6-fluoro-8-methoxy-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid ethyl ester preparation of

[0059] Add 100g of ethyl 1-cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxo-3-quinolinecarboxylate into the three-necked flask, and then add 600mL of DMF to it: DMSO=1:1 mixed solvent, stir, add 62.2mL of 2,3,4-trimethoxybenzylamine, raise the temperature to 120°C for 6h, cool down, pour the reaction solution into 1mol / L dilute hydrochloric acid, stir, add Extract with 500mL EA, separate the organic layer, extract the aqueous phase with 300mL×2 EA, combine the organic layers, dry, filter and evaporate to dryness to obtain 92.3g of a yellow product, which is directly used in the next step without purification.

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Abstract

The invention discloses a preparation method and a detecting method of a moxifloxacin hydrochloride photodegraded impurity and an application of the moxifloxacin hydrochloride photodegraded impurity as an impurity reference substance during detection of a moxifloxacin hydrochloride related substance. Through the preparation of the compound, the reference substance is provided for analysis of the moxifloxacin hydrochloride related substance, so as to improve the quality standard of moxifloxacin hydrochloride, and provide important guidance significance for safe medication of moxifloxacin hydrochloride.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a preparation method, detection method and application of moxifloxacin hydrochloride photodegradable impurities. Background technique [0002] Moxifloxacin hydrochloride (moxifloxacin hydrochloride, 1-cyclopropyl-7-(S,S-2,8-diazo-bicyclo[4.3.0]nonan-8-yl)-6-fluoro-8-methanol Oxy-1,4-dihydro-4-oxo-3-quinoline carboxylic acid hydrochloride) is the fourth-generation quinolone antibacterial drug developed by Bayer, Germany, which was first listed in Germany in September 1999. A broad-spectrum antimicrobial commonly used clinically, it has the characteristics of broad-spectrum, high efficiency, low drug resistance, low toxicity, etc., and its structural formula is as follows: [0003] [0004] Photochem.Photobiol.Sci.2012, 11, 351 has publicly reported that during the stability experiment, moxifloxacin hydrochloride is prone to photolysis reaction, resulting in impur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/56G01N30/02
CPCC07D215/56G01N30/02G01N2030/027
Inventor 王足兵赵超郭璇柴雨柱朱谧徐丹杨治旻田舟山
Owner NANJING CHIA TAI TIANQING PHARMA
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