A kind of purification method of warnemulin salt

A Vonimulin and purification method technology, applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve the problems of physical injury to operators, unfavorable industrial production, flammable and explosive ethers, etc. The effect of low energy consumption cost of raw materials, reduction of the use of flammable and explosive solvents, and low cost of toxicity

Active Publication Date: 2016-08-17
ZHEJIANG ESIGMA BIOTECH CO LTD
View PDF5 Cites 0 Cited by
  • 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 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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

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%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap