Refining method of marbofloxacin

A refining method and technology of marbofloxacin, applied in the direction of organic chemistry, etc., can solve the problems affecting bioavailability, solubility, pharmacological safety, irregular crystal form, non-crystalline form, etc., to improve bioavailability and pharmacological safety. properties, improve purity and content, improve appearance and color

Inactive Publication Date: 2017-08-18
山东方明邦嘉制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the marbofloxacin currently produced generally has problems such as high impurities, irregular color, crystal form or non-crystal form, which affect bioavailability, solubility, pharmacological safety, etc.

Method used

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  • Refining method of marbofloxacin
  • Refining method of marbofloxacin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add 10g of crude marbofloxacin to a 250ml three-necked flask, then add 45ml of water, stir at room temperature until there are no obvious particles, then add 2.2g of formic acid, and stir for 20min. Suction filtration to collect filter cake.

[0023] (2) Add 60ml of isopropanol and 20ml of water into a 250ml three-necked flask, then add the filter cake to suspend the filter cake in the mixed solvent, then add DIEA to adjust the pH to 8.0, stir to dissolve, add activated carbon, and heat up to reflux at 60°C 20min-40min, filter and collect the filtrate

[0024] (3) Add the filtrate to a 250ml three-neck flask, slowly heat up, and start to concentrate. When the temperature reaches 83°C, naturally cool down to 25°C, continue to cool down and crystallize to 8°C, continue to keep warm for 20 minutes, suction filter, wash, vacuum 60 After drying at ℃, 8.53 g of marbofloxacin fine product was obtained.

Embodiment 2

[0026] (1) Add 10g of crude marbofloxacin to a 250ml three-necked flask, then add 50ml of water, stir at room temperature until there are no obvious particles, then add 3.9g of acetic acid, and stir for 20min. Suction filtration to collect filter cake.

[0027] (2) Add 75ml of ethanol and 26.5ml of water into a 250ml three-necked flask, then add the filter cake, suspend the filter cake in the mixed solvent, then add ammonia water to adjust the pH to 8.5, stir to dissolve, add activated carbon, heat up and reflux at 60°C for 20min -40min, filter, collect filtrate

[0028] (3) Add the filtrate to a 250ml three-neck flask, slowly heat up, and start to concentrate. When the temperature reaches 81°C, naturally cool down to 20°C, continue to cool down and crystallize to 5°C, continue to keep warm for 20 minutes, filter, wash, and vacuum 60°C After drying at ℃, 9.02 g of marbofloxacin fine product was obtained.

Embodiment 3

[0030] (1) Add 10g of crude marbofloxacin to a 250ml three-neck bottle, then add 50ml of water, stir at room temperature until there are no obvious particles, then add 3g of formic acid, and stir for 20min. Suction filtration to collect filter cake.

[0031] (2) Add 70ml of methanol and 25ml of water into a 250ml three-necked flask, then add the filter cake to suspend the filter cake in the mixed solvent, then add triethylamine to adjust the pH to 8.5, stir to dissolve, add activated carbon, and heat up to reflux at 60°C 20min-40min, filter and collect the filtrate

[0032] (3) Add the filtrate to a 250ml three-necked flask, slowly heat up, and start to concentrate. When the temperature reaches 75°C, naturally cool down to 20°C, continue to cool down and crystallize to 5°C, continue to keep warm for 20 minutes, filter, wash, and vacuum 60°C ℃ drying, to obtain 8.13 grams of marbofloxacin fine.

Description of drawings

[0033] figure 1 It is the high performance liquid c...

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Abstract

The invention discloses a refining method of marbofloxacin. The refining method comprises the following steps of (1) dissolving a marbofloxacin crude product in a certain amount of water, stirring until no obvious particles exist, then adding a certain amount of acid, stirring for 20min to 30min, and carrying out suction filtration; (2) dissolving a filter cake in a certain amount of solvent or mixed solvent, adding alkali to adjust PH to 7.0 to 9.0, stirring for clarifying, adding activated carbon, warming at the temperature of 40 DEG C to 60 DEG C, reflowing for 20min to 40min, filtering, and collecting a filter liquor; (3) concentrating the filter liquor, after concentrating to a certain temperature, starting to cool to 20 DEG C to 30 DEG C, continuously cooling to 0 DEG C to 10 DEG C, keeping warm for 30min to 50min, carrying out suction filtration, washing and drying.

Description

technical field [0001] The invention relates to a method for refining marbofloxacin Background technique [0002] Marbofloxacin is a third-generation fluoroquinolone drug specially developed for animals developed by Vétoquinol. It has broad-spectrum anti-infection and has antibacterial effects on Gram-negative bacteria, Gram-positive bacteria and mycoplasma. It is used to treat deep and Superficial skin infection, urinary tract infection, skin and soft tissue infection in cats, acute upper respiratory tract infection. Marbofloxacin has outstanding pharmacological characteristics: long elimination half-life (10-12 hours for dogs, 8-10 hours for cats), and nearly 100% bioavailability. Since Marbofloxacin was first launched in 1995, the number of countries, indications, applicable animals, and dosage forms in 1998 and 1999 have been continuously increasing. From the analysis of veterinary antibacterial drugs approved and marketed abroad, marbofloxacin is the most promising ve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/06
CPCC07D498/06
Inventor 孙建林国鹏
Owner 山东方明邦嘉制药有限公司
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