A kind of purification method of warnemulin salt

Abstract

The present invention relates to a kind of method that purifies and produces solid warnemulin salt fine product from the crude product of warnemulin salt: (1) get the aqueous solution of the warnemulin salt that concentration is 1-15wt%, add alkali to adjust pH to 7-14, filter, add solvent I to wash, and filter cake is dried to obtain warnemulin base, and described solvent I is water or low-concentration methanol solution or ethanol solution or isopropanol solution; (2) step (1) ) to dissolve the obtained warnemulin base in solvent II, drop into water under stirring, and obtain the fine product of warne muulin base through crystallization, filtration, washing and drying. The solvent II is methanol, ethanol, isopropanol, normal Butanol or other alcoholic solvents, the volume of described solvent II is 5-100 times of the mass of warnimulin base, preferably 10-20 times of volume; Add it into the acid solution, and dry it after the reaction is complete to obtain the pure solid product of warnemulin salt. The invention has the advantages of simple process, easy realization of production, low cost, no pollution and high 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