Crystallization method of valnemulin hydrochloride

A technology for the crystallization of warnemulin hydrochloride, which is applied in the field of crystallization of warnemulin hydrochloride, can solve the problems of equipment corrosion, high energy consumption, and no purification effect of the product, and achieve simple operation and low cost Effect

Active Publication Date: 2011-10-26
ZHEJIANG GUOBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But above-mentioned two kinds of methods all have obvious limitation: first, these two kinds of methods are only a process of removing solvent, have no purifying effect to product, therefore very high to the content requirement of vonemulin hydrochloride aqueous solution; Secondly, the aqueous solution of varnemulin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 10.0g (0.0177mol) of vonemulin (HPLC content: 95.0%), completely dissolve it in 100mL of methyl tert-butyl ether, cool to 0°C, add 21.7g of hydrogen chloride in methanol solution (containing 6.5% hydrogen chloride) dropwise under stirring g, 0.178mol), after the dropwise addition, stir for 2 hours, filter under reduced pressure, rinse the filter cake with an appropriate amount of methyl tert-butyl ether, dry, and get 10.1g of Devornimulin hydrochloride (yield 94.9%, HPLC Content 98.2%).

Embodiment 2

[0023] Take 10.0g (0.0177mol) of vonemulin (HPLC content: 95.0%), completely dissolve it in 100mL of dichloromethane, cool to -20°C, slowly add 0.65g (0.0178mol) of dry hydrogen chloride under stirring, and pass through , stirred for 2 hours, filtered under reduced pressure, rinsed the filter cake with an appropriate amount of methyl tert-butyl ether, and dried to obtain 7.8 g of vornimulin hydrochloride (yield 73.3%, HPLC content 96.5%).

Embodiment 3

[0025] Take 10.0g (0.0177mol) of vonemulin (HPLC content: 95.0%), completely dissolve it in 100mL of toluene, raise the temperature to 40°C, slowly pass in 12.9g (0.353mol) of dry hydrogen chloride under stirring, and stir for 2 hour, filter under reduced pressure, rinse the filter cake with an appropriate amount of methyl tert-butyl ether, and dry to obtain 9.0 g of Devornimulin hydrochloride (yield 84.6%, HPLC content 96.8%).

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PUM

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Abstract

The invention mainly discloses a crystallization method of valnemulin hydrochloride. The method comprises the following steps: dissolving valnemulin in an organic solvent; adding a certain amount of dried hydrogen chloride gas or hydrogen chloride organic solution; separating out crystals; and collecting the obtained crystals, and drying so as to obtain valnemulin hydrochloride. The method is convenient for operation, is suitable for industrial production on large scale, has low cost and can be used for purifying the product. The chromatograph content of the valnemulin hydrochloride obtained by the method in the invention is improved by 1-5% as compared with the chromatograph content of the corresponding valnemulin.

Description

technical field [0001] The invention provides a crystallization method of warnemulin hydrochloride. Background technique [0002] Valnemulin is a second-generation pleuromutilins semi-synthetic antibiotic for animals. It belongs to terpenes and belongs to the same class of drugs as tiamulin. It is mainly used to prevent mycoplasma disease and Gram-positive bacterial infection in pigs, cattle, sheep and poultry. In 1984, Sandoz Company first used pleuromutilin as a semi-synthesized antibiotic. [0003] Because of the instability of warnemulin, it is generally used clinically as a premix of warnemulin hydrochloride. In 1999, Warnemulin hydrochloride premix was first listed in the United States under the trade name of Econor. It is also the first veterinary drug premix approved in Europe and listed as a prescription drug for veterinary use. [0004] US5164526 uses the spray drying method to prepare the solid of warnemulin hydrochloride; CN101597248 and CN101735123 both use ...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/28
Inventor 邱家军杨训付君平姚礼高侯仲轲王霞韩利华
Owner ZHEJIANG GUOBANG PHARMA
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