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Method for preparing high-purity nemadectin

A high-purity technology for nemoctine, applied in the field of preparation of high-purity nemoctine, can solve the problems of difficult application, expensive macroporous adsorption resin, worrying service life, etc., and achieve a highly targeted effect

Active Publication Date: 2014-02-19
DALIAN JOIN KING FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The macroporous adsorption resin used in this method is expensive and difficult to apply in industrial production; and this method lacks protection for the macroporous adsorption resin used, and its service life is worrying

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put 1.0kg of dried mycelia of nimoctine (in which the external standard content of nimoctine is 5.5%) and 6.0kg of 55% ethanol aqueous solution into a 10L kettle, and stir at 23°C for 4 hours. Filter to obtain 4.84kg of brown filtrate; return the filter cake to the kettle, add 6.0kg of 55% ethanol aqueous solution and continue to stir for 4 hours. Filter to obtain 6.15kg of light brown filtrate. The two filtrates were combined, in which the external standard content of nemoctine was 0.50%, and the purity was 58.4%.

[0017] The extract is put on the decolorization column, the resin is FPA53 (Rohm and Haas, adsorption capacity 30 g ~ 40 g / L), and the flow rate is 2.0 L / h. The effluent is light yellow transparent solution.

[0018] Macroporous adsorption resin 1 and macroporous adsorption resin 2 on the decolorizing solution. Among them, the macroporous adsorption resin 1 is XAD1180N (Rohm and Haas), and the dosage is 0.5L; the macroporous adsorption resin 2 is XAD1600...

Embodiment 2

[0020] Put 1.0kg of dried mycelia of nimoctine (in which the external standard content of nimoctine is 5.5%) and 8.0kg of 50% ethanol aqueous solution into a 10L kettle, and stir at 20°C for 6 hours. Filter to obtain 7.78kg of brown filtrate; return the filter cake to the kettle, drop in 8.0kg of 50% ethanol aqueous solution and continue to stir for 6 hours. Filter to obtain 8.31kg of light brown filtrate. The two filtrates were combined, and the external standard content of nemoctine was 0.34%, and the purity was 58.6%.

[0021] The extract is put on the decolorization column, and the resin is DOC2001 (Suqing resin, the adsorption capacity is 30 g ~ 40 g / L), and the flow rate is 3.0 L / h. The effluent is light yellow transparent solution.

[0022] Macroporous adsorption resin 1 and macroporous adsorption resin 2 on the decolorizing solution. Among them, the macroporous adsorption resin 1 is XAD1180N (Rohm and Haas), and the dosage is 0.8L; the macroporous adsorption resin 2...

Embodiment 3

[0024] Put 1.0kg of dried mycelia of nimoctine (in which the external standard content of nimoctine is 5.5%) and 5.0kg of 60% ethanol aqueous solution into a 10L kettle, and stir at 21°C for 4 hours. Filter to obtain 3.88 kg of brown filtrate; return the filter cake to the kettle, drop in 5.0 kg of 60% ethanol aqueous solution and continue to stir for 4 hours. Filter to obtain 5.20kg of light brown filtrate. The two filtrates were combined, and the external standard content of nemoctine was 0.61%, and the purity was 57.9%.

[0025] The extract is put on the decolorization column, the resin is FPA40 (Rohm and Haas, the adsorption capacity is 30 g ~ 40 g / L), and the flow rate is 1.2 L / h. The effluent is light yellow transparent solution.

[0026] Macroporous adsorption resin 1 and macroporous adsorption resin 2 on the decolorizing solution. Among them, the macroporous adsorption resin 1 is H60 (Xi’an Electric Power), and the dosage is 0.4L; the macroporous adsorption resin 2 ...

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Abstract

The invention discloses a method for preparing high-purity nemadectin and belongs to the field of medicinal chemistry. The nemadectin is a sixteen-member macrolide type anthelmintic antibiotic and mainly used for synthesizing moxidectin with the better anthelmintic effect. According to the method for preparing the high-purity nemadectin, the nemadectin is extracted through an ethanol-water solution, and an extract is obtained, decolorized through ion exchange resin, deproteinized and desugared through macroporous adsorption resin and finally adsorbed and separated through the appropriate macroporous adsorption resin, so that nemadectin products with the purity higher than 90% can be prepared. The method is high in pertinency through matched usage of the resin, and the prepared high-purity nemadectin has great significance in synthesis of the high-purity moxidectin.

Description

technical field [0001] The invention relates to a method for preparing high-purity nemoctine, which belongs to the field of medicinal chemistry. Background technique [0002] Nimoctine is a sixteen-membered macrolide anthelmintic antibiotic, which can be used to treat internal and external parasites in animals such as cattle and sheep. Nimoctine is fermented by Streptomyces couscous, and it is mainly used to synthesize moxictine with better efficacy. Therefore, high-purity nemoctine is of special significance for the preparation of high-purity moxictine. [0003] There are fewer methods for purifying nimoctine reported in the known literature, and there are mainly the following two types: [0004] 1. Chinese patent CN101372492A discloses a method for purification by macroporous adsorption resin column chromatography. The purity of nemoctine obtained by this method is 40%-50%, and further column chromatography purification is required in the process of synthesizing moxicti...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 杜志博王维新梁全德赵丹阳赵欢王荣良戚元强
Owner DALIAN JOIN KING FINE CHEM CO LTD
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