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Method for purifying valnemulin hydrochloride

A technology of nemoline hydrochloride and its purification method, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as difficult purification of valnemulin hydrochloride, and achieve avoidance of re-extraction, Ease of waste water and less product loss

Active Publication Date: 2012-02-08
浙江拜克生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The present invention provides an effective and stable method for purifying valnemulin hydrochloride, which has a simple and convenient treatment process, does not require multiple extractions of valnemulin salt and the introduction of other salts, has less product loss, and is easy to treat waste water , solved the problem of difficult purification of valnemulin hydrochloride

Method used

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  • Method for purifying valnemulin hydrochloride
  • Method for purifying valnemulin hydrochloride
  • Method for purifying valnemulin hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Accurately weigh 64.6 g of valnemulin hydrochloride with a content of 80% and dissolve it in 600 ml of water, add 600 ml of dichloromethane, adjust the pH to 8.2 with aqueous sodium hydroxide solution, let stand for layers, discard the water layer, and discard the organic layer After washing with 600ml of water, it was vacuum-dried. Add 200ml of methanol to the dried solid and dissolve it completely, then add 84.2g of 10% phosphoric acid, stir for 0.5h, evaporate to dryness, then add 100ml of methanol to dissolve again. To the obtained methanol solution, slowly add 1100ml of methyl tert-butyl ether dropwise under vigorous stirring and stir until the precipitation is complete, filter, wash the filter cake with a small amount of dichloromethane, and distill the filtrate to recover the solvent for reuse. Dissolve the filter cake with 1200ml of methyl tert-butyl ether / water mixed solution with a volume ratio of 1 / 1, adjust the pH to 7.2 with lye, let the layers stand and di...

Embodiment 2

[0037]Accurately weigh 80g of 85% valnemulin sulfate, dissolve it in 960ml of water, add 960ml of methyl tert-butyl ether, adjust the pH to 9.0 with potassium hydroxide aqueous solution, let it stand for stratification, discard the water layer, organic The layer was washed with 960 ml of water and vacuum-dried. Add 230ml of ethanol to the dry solid and dissolve it completely, add 50.2g of 20% phosphoric acid, stir for 0.5h, evaporate to dryness, then add 120ml of ethanol to redissolve. To the obtained ethanol solution, slowly add 1400ml of methyl tert-butyl ether dropwise under vigorous stirring and stir until the precipitation is complete, filter, and wash the filter cake with a small amount of methyl tert-butyl ether, and the filtrate is rectified to recover ether and methanol respectively reuse. Dissolve the filter cake with 1600ml of methyl tert-butyl ether / water mixed solution with a volume ratio of 1 / 1, adjust the pH to 8.0 with lye; let stand to separate layers, discar...

Embodiment 3

[0039] Accurately weigh 100 g of valnemulin tartrate with a content of 90% and dissolve it in 1000 ml of water, add 1000 ml of a mixed solvent of n-hexane and petroleum ether with a volume ratio of 1:1, adjust the pH to 8.0 with ammonia water, let stand and separate, The aqueous layer was discarded, and the organic layer was washed with 1000 ml of water and dried under reduced pressure. Add 400ml of methanol to the dried solid and dissolve it completely, then add 41.1g of 30% phosphoric acid, stir for 0.5h, evaporate to dryness, then add 100ml of methanol to dissolve again. To the resulting methanol solution, slowly add 1000ml of a mixed solution of n-hexane and petroleum ether with a volume ratio of 1:1 dropwise under vigorous stirring and stir until the precipitation is complete, filter, and wash the filter cake with a small amount of petroleum ether Recover solvent and methanol. Dissolve the filter cake with 2000ml of methyl tert-butyl ether / water mixed solution with a vol...

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Abstract

The invention provides a method for purifying valnemulin hydrochloride. The method comprises the following steps of: directly alkalizing crude valnemulin in an aqueous solution thereof; and directly preparing into phosphate in an alcohol solution and curing. In the method, multiple times of extraction of valnemulin hydrochloride and introduction of other salts are not required, the treating process is easy and convenient, the loss of the product is small, waste water is easy to treat, and the problem of difficulty in purifying the valnemulin hydrochloride is solved.

Description

technical field [0001] The invention relates to a method for purifying valnemulin salt, in particular to a method for purifying valnemulin hydrochloride. Background technique [0002] Valnemulin, as a new generation of pleuromutilin semi-synthetic antibiotics, is mainly used for the prevention and treatment of mycoplasma and gram-positive bacterial infections in pigs, cattle, sheep and poultry. Valnemulin can bind to the 50S subunit of the ribosome of pathogenic microorganisms and inhibit protein synthesis, and its mechanism of action is similar to that of tiamulin. Valnemulin has the characteristics of strong antibacterial activity, broad spectrum, fast absorption, short drug withdrawal period, no reproductive toxicity, safety, and extremely low residue. Valnemulin is effective against mycoplasma, bacteria and spirochetes, such as Mycoplasma arthritis, Mycoplasma bovis, Mycoplasma canis, Mycoplasma felis, Mycoplasma gallisepticum, Mycoplasma gallisepticum, Mycoplasma pneum...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/28
Inventor 葛庆余罗晓芳李大娟余炜唐显重方明山
Owner 浙江拜克生物科技有限公司
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