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A kind of purification method of tiamulin reaction liquid in industrial production

A tiamulin and purification method technology, applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve the problems of complexity, high cost, complex tiamulin production process, etc., and achieve simplified purification method , the effect of reducing production costs

Active Publication Date: 2014-10-22
大英九合药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such complicated post-treatment steps of the reaction solution make the production process of tiamulin complex and costly

Method used

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  • A kind of purification method of tiamulin reaction liquid in industrial production
  • A kind of purification method of tiamulin reaction liquid in industrial production
  • A kind of purification method of tiamulin reaction liquid in industrial production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] According to the method for synthesizing tiamulin in U.S. Patent US4278674 and British Patent GB1410505, and the corresponding raw materials, catalyst and solvent proportioning, pleuromutilin p-toluenesulfonate ester of 106 grams (1.0 moles) and equimolar 2- Diethylaminoethanethiol hydrochloride was reacted, and the solid obtained by concentrating was dissolved in 850 ml of ethyl acetate, washed with water (500 ml × 2), and the reaction solution was neutralized to pH6.7 with 10% phosphoric acid. Then it was washed with water (300 ml×2) to obtain a tiamulin-ethyl acetate solution with a chromatographic purity of 98.5%. The solution can be directly used to react with fumaric acid to synthesize tiamulin fumarate.

Embodiment 2

[0020] According to the method for synthesizing tiamulin in U.S. Patent US4278674 and British Patent GB1410505, and the corresponding raw materials, catalyst and solvent proportioning, pleuromutilin p-toluenesulfonate ester of 106 grams (1.0 moles) and equimolar 2- Diethylaminoethanethiol hydrochloride was reacted, and the concentrated obtained solid was dissolved in 800 ml of ethyl acetate, then after washing with water (500 ml × 2), the reaction solution was neutralized to pH7.0 with 10% phosphoric acid , and then washed with water (300 ml×2), to obtain a tiamulin-ethyl acetate solution with a chromatographic purity of 98.0%. The solution can be directly used to react with fumaric acid to synthesize tiamulin fumarate.

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Abstract

The invention relates to a purification method for a tiamulin reaction solution in industrial production. Specifically, the method includes: in a purification process of a tiamulin reaction solution, firstly using water to wash off water soluble impurities, i.e. p-toluene sulfonic acid and an alkaline catalyst from the tiamulin reaction solution, then adjusting the pH value of the tiamulin reaction solution to 6.7-7.0 with phosphoric acid, selectively making the organic impurity 2-diethylaminoethanethiol therein acidified into a salt, then using water to wash 2-diethylaminoethanethiol phosphate away from the tiamulin reaction solution, thus obtaining a tiamulin-ethyl acetate solution with chromatographic purity of 98-98.5% of. The method has the advantages of simple purification process and low cost.

Description

1. Technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a method for purifying a tiamulin reaction liquid in industrial production, especially in the process of purifying the tiamulin reaction liquid, first washing the tiamulin reaction liquid with water water-soluble impurities, then use phosphoric acid to adjust the pH value of the organic phase of the tiamulin reaction solution, selectively acidify the organic impurities 2-diethylaminoethanethiol into a salt, and then react with water from the tiamulin Washed away in the solution to achieve the purpose of purifying the pure tiamulin reaction solution. 2. Background technology [0002] Tiamulin (1) is an organic base: [0003] [0004] After it forms a salt with fumaric acid, tiamulin fumarate (2) is obtained: [0005] [0006] Tiamulin fumarate is an important veterinary drug, which is mainly used for the prevention and treatment of chicken chronic respiratory disea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/52C07C319/28
Inventor 穆万勇刘忠东
Owner 大英九合药业有限公司
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