Purification method of valnemulin salt

A technology of varnimulin and purification method, which is applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve the problems of physical injury of operators, unfavorable industrial production, increase of solvent residue, etc., and achieve raw material energy Low consumption cost, reduce the use of flammable and explosive solvents, and produce extremely easy effects

Active Publication Date: 2014-12-24
ZHEJIANG ESIGMA BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The Chinese invention patent with the publication number CN103483232A discloses a refining method of warnemulin hydrochloride, that is, the method of dissolving and recrystallizing with ethers, but this method introduces a variety of solvents during the preparation process, increasing the amount of solvent in the product. Residues, and ethers are flammable and explosive, pollute the environment, and have certain har

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 200 ml of an aqueous solution of warnemulin hydrochloride (containing 20 grams of warnemulin hydrochloride), adjust the pH to 9.3 with 10N sodium hydroxide solution; filter the precipitate, dry the filter cake and dissolve it in 200 ml of ethanol During the process, start stirring, and add 200 milliliters of water dropwise. After the dropwise addition, continue to stir for 60 minutes, filter, wash the filter cake with a small amount of 50% ethanol solution, and dry to obtain the fine product of warnimulin base.

[0031] Add the obtained warnemulin base into water, adjust the pH of the reaction system to 4.5 with 6N hydrochloric acid solution, stir for 30 minutes until the warnemulin base is completely dissolved, and spray-dry the solution to obtain a solid of warnemulin hydrochloride Product 19.3 grams, purity: 99.2%, moisture: 1.2%, solvent residual 0.021%.

Embodiment 2

[0033] Take 500 ml of an aqueous solution of warnemulin hydrochloride (containing 50 grams of warnemulin hydrochloride) and adjust the pH to 9.0 with 8N sodium hydroxide solution. The precipitate was filtered, and the filter cake was dried and dissolved in 500 ml of methanol, started to stir, and 500 ml of water was added dropwise, after the dropwise addition, continued to stir for 30 minutes, filtered, and the filter cake was washed with a small amount of 40% methanol solution and dried. Get Warnemulin Premium.

[0034] Add the obtained warnemulin base into water, adjust the pH of the reaction system to 4.3 with 5N hydrochloric acid, stir for 30 minutes until the warnemulin base is completely dissolved, and spray-dry the solution to obtain a solid product of warnemulin hydrochloride 48.2 grams, purity: 98.8%. , Moisture: 1.5%, residual methanol 0.024%.

Embodiment 3

[0036] 1000 ml of an aqueous solution of warnemulin hydrochloride (containing 105.2 grams of warnemulin hydrochloride) was used to adjust the pH to 8.7 with 10N sodium hydroxide solution. The precipitate is filtered, and the filter cake is dried and dissolved in 1000 ml of isopropanol. Stirring is started, and 950 ml of water is added dropwise. After the dropwise addition, continue to stir for 30 minutes, and filter. After washing and drying, the fine product of warnimulin is obtained.

[0037] Add the obtained warnemulin base into water, adjust the pH of the reaction system to 4.7 with 6N hydrochloric acid, stir for 60 minutes until the warnemulin base is completely dissolved, and spray-dry the solution to obtain a solid product of warnemulin hydrochloride 998.6 grams, purity: 99.1%, moisture: 1.6%, isopropanol residual 0.025%.

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Abstract

The invention relates to a method for preparing a solid valnemulin salt refined product by purifying a valnemulin salt crude product, which comprises the following steps: (1) taking a 1-15 wt% valnemulin salt water solution, adding alkali to regulate the pH value to 7-14, filtering, adding a solvent I for washing, and drying the filter cake to obtain a valnemulin alkali, wherein the solvent I is water or a low-concentration methanol solution or ethanol solution or isopropanol solution; (2) adding the valnemulin alkali obtained in the step (1) into a solvent II, dissolving, dropwisely adding water while stirring, crystallizing, filtering, washing and drying to obtain a valnemulin alkali refined product, wherein the solvent II is methanol, ethanol, isopropanol, n-butanol or any other alcohol solvent, and the volume of the solvent II is 5-100 times of the mass of the valnemulin alkali and preferably 10-20 times; and (3) adding the valnemulin alkali refined product obtained in the step (2) into an acid solution, reacting completely, and drying to obtain the pure valnemulin salt solid product. The method has the advantages of simple technique, practical production, low cost, no pollution and higher yield.

Description

technical field [0001] The invention relates to a preparation method of warnemulin salt, in particular to a method for purifying a solid warnemulin salt fine product from a crude product of warnemulin salt. Background technique [0002] Pleuromutilin derivatives are broad-spectrum bimectin antibiotics, which have good antibacterial activity against a variety of Gram-positive bacteria and a variety of mycoplasma and spirochetes. Pleuromutilin chemical derivatives mainly include tiamulin, warnimulin and the human antibiotic retapalene. As a veterinary antibiotic, the domestic production process is mainly to use Pleuromutilus or Basidiomycetes to ferment and produce the fermentation liquid containing pleuromutilin. The pleuromutilin synthetic derivative salt is obtained through pretreatment, extraction, synthesis, spray drying and other processes of the fermentation liquid. [0003] Valnemulin is a new generation of pleuromutilin (Pleuromutilin) ​​semi-synthetic antibiotics,...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/28
Inventor 黄振徐天华王丽陈军吴中华何奇雷
Owner ZHEJIANG ESIGMA BIOTECH CO LTD
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