Purification method of valnemulin salt

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,...

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 harm to the operator's body

Chinese patent CN101456833 discloses a method for purifying warnemulin hydrochloride. After the method adopts warnemulin and ketone to react, deprotection, so as to achieve the purpose of purifying warnemulin hydrochloride, but the method steps are more loaded down with trivial details, not It is beneficial to industrial production, and the yield is greatly reduced after increasing the reaction steps