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Preparation method of fumaric acid valnemulin

A technology of fumaric acid and methyl isobutyl ketone, applied in the field of preparation of medicinal chemicals, can solve the problems of increasing the cost of final products, inaccurate dosage of animal medicines, low storage stability and the like

Inactive Publication Date: 2011-09-14
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Loss of active ingredient undoubtedly results in inaccurate dosing of animals, leading to questions about the success of the treatment and a substantial increase in the cost of the final product
[0007] It has been shown that the storage stability of warnemulin as a monomer in granules is much lower than that in dry or amorphous hydrochloride form

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 7ml of methyl isobutyl ketone into the reaction bottle, conduct a constant temperature water bath, control the temperature at 65-70°C, then add 0.5g of warnemulin, and stir until the solution is clear. Keep the temperature constant, continue to add 1.5ml of absolute ethanol, add 0.13g of fumaric acid under stirring, and control the reaction time for 2 hours. After the end of the reaction, keep warm in an ice bath for 3 hours. Filter, wash with methyl isobutyl ketone, and dry to obtain 0.44 g of warnimulin fumarate.

Embodiment 2

[0025] Add 14ml of methyl isobutyl ketone into the reaction bottle, conduct a constant temperature water bath, and control the temperature at 65-70°C, then add 1g of warnemulin, and stir until the solution is clear. Keep the temperature constant, continue to add 4ml of anhydrous methanol, add fumaric acid 0.27g under stirring, and control the reaction time for 2 hours. After the end of the reaction, keep warm in an ice bath for 3 hours. Filter, wash with methyl isobutyl ketone, and dry to obtain 0.86 g of warnimulin fumarate.

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PUM

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Abstract

The invention relates to a preparation method of fumaric acid valnemulin. The preparation method comprises the following steps: firstly adding valnemulin in a methyl isobutyl ketone solution, then heating and stirring; after dissolving, adding absolute ethanol, adding fumaric acid until a reaction solution is clear; reducing the temperature with ice bath so as to separate out crystal; filtering, and washing filter cake with methyl isobutyl ketone; and drying so as to obtain the fumaric acid valnemulin, wherein the melting point of the fumaric acid valnemulin is larger than 130 DEG C, and the yield of the fumaric acid valnemulin reaches 85%.

Description

technical field [0001] The invention relates to a preparation method of medicinal chemicals, in particular to a preparation method of vonemulin fumarate. Background technique [0002] Vernimulin is a new generation of pleuromutilin semi-synthetic antibiotics, which belongs to diterpenes and is a special antibiotic for animals. In 1984, it was first synthesized by Berner H of Sandoz Company using pleuromutilin as a raw material. Later, Norvatis used it as a premix under the trade name Econor, which is now on the market in many countries. Warnimulin is mainly used for the prevention and treatment of mycoplasma disease and Gram-positive bacterial infection in pigs, cattle, sheep and poultry. In 1999, it was approved by the European Community for the prevention and treatment of swine dysentery caused by Brachyspira hyodysenteriae infection and swine enzootic pneumonia caused by Mycoplasma pneumoniae infection. It is the first European-wide approved veterinary drug premix, lis...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/20C07C57/15C07C51/41
Inventor 吴汝林王繁业
Owner QINGDAO UNIV OF SCI & TECH
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