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Preparation method of tiamulin alkali

A technology for tiamulin and pleuromutilin, which is applied in the fields of thioether preparation and organic chemistry, and can solve the problems of restriction, foul smell, and restriction of tiamulin base production, etc.

Inactive Publication Date: 2013-05-22
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The biggest problem in this process is the use of 2-diethylaminoethanethiol. 2-Diethylaminoethanethiol has a foul smell. Its a

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Preparation of Pleuromutilin Thiourea Salt

[0021] Put 20g of pleuromutilin and 40ml of chloroform into the reaction bottle, add 2.5ml of thionyl chloride, carry out chlorination reaction at 35°C for 2 hours, then add 5.4g of thiourea and continue the reaction for 3 hours to obtain pleuromutilin thiourea salt solution.

Embodiment 2

[0023] Preparation of tiamulin base

[0024] In the reaction bottle, add ethyl acetate, then add 8ml of 2-diethylaminoethanol and 2ml of thionyl chloride, and react at room temperature for 1 hour. The obtained reaction liquid was mixed with pleuromutilin thiourea salt solution, and reacted at 48° C. for 4 hours. Dry over anhydrous sodium sulfate and evaporate the solvent to obtain tiamulin base with a yield of 90.9%.

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PUM

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Abstract

The invention relates to a preparation method of tiamulin alkali. The preparation method comprises the following steps of: adding pleuromutilin in a chlorinating agent in a solvent for chlorinating, and then adding thiourea for reacting to obtain a solution; chlorinating 2-diethylaminoethanol in the solvent by using the chlorinating agent to obtain a chloride solution of 2-diethylaminoethanol; and mixing two solutions together to react, controlling the reaction temperature and reaction time, dewatering and drying the obtained product, and evaporating the solvent so as to obtain tiamulin alkali. The yield of tiamulin alkali can be more than 80%. The reaction method for preparing tiamulin alkali is simple and easy to control; and 2-diethylaminoethanethiol which has fetid smell and is limited application is abolished, so that the preparation method has a good commercial prospect.

Description

technical field [0001] The invention relates to a preparation method of medicinal chemicals, in particular to a preparation method of tiamulin base. Background technique [0002] Tiamulin base is a semi-synthetic diterpene compound, which is a special antibiotic for livestock and poultry. Tiamulin base is rapidly absorbed in animals, with high blood concentration, wide distribution in the body, and low residue. It has good curative effect on mycoplasma infection of pigs and poultry, porcine treponema dysentery, and staphylococcal synovitis of chicken, and has growth-promoting effect, so it is widely used as veterinary medicine and feed additive. [0003] At present, the production process commonly adopted by manufacturers is to synthesize tiamulin base by reacting with 2-diethylaminoethanethiol in a solvent under controlled conditions after obtaining pleuromutilin through fermentation and culture. [0004] The biggest problem in this process is the use of 2-diethylaminoeth...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/20
Inventor 吴汝林吴广启王凡业
Owner QINGDAO UNIV OF SCI & TECH
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