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Method for purification of milbemycins

A kind of technology of acaricid and refining method, applied in the direction of organic chemistry, etc., can solve the problems of low productivity, low carrier load, high cost of refined products, etc.

Active Publication Date: 2006-02-08
MITSUI CHEM AGRO INC
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Problems solved by technology

[0006] As a general purification method of the above-mentioned compound, it is known that the above-mentioned compound is extracted from the fermentation culture with an organic solvent, and then purified by using silica gel, alumina, dextran gel, ion exchange resin, synthetic adsorbent, molecular sieve, C 8 h 17 、C 8 h 37 、C 6 h 5 Chromatography using chemically bonded silica gel or the like as a carrier to obtain a fraction containing the target compound, and concentrate and solidify it (for example, refer to Patent Document 1, Patent Document 2, Patent Document 3, and Patent Document 4), but these use chromatographic method, the carrier load is low, so it is necessary to use a large amount of chromatographic carriers and organic solvents and other stripping solvents, the productivity is also low, and the cost of the resulting refined product is high, so it is not necessarily a refining method that meets industrial needs.

Method used

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  • Method for purification of milbemycins

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Embodiment 1

[0043] Mitetoxin A 3 and acaricidin A 4 Ethyl acetate solution was prepared from the residue of the fermentation broth. As a result of concentrating a part under reduced pressure, it was found that the concentration residue had a purity of 28% (Acaricidin A 3 : 4.2%; Acaricidin A 4 : 23.8%). This ethyl acetate solution (130 ml) was washed successively with 63 ml of 5% aqueous ammonia and 39 ml of 5% aqueous sulfuric acid. To the residue obtained by concentrating the ethyl acetate solution, 300 ml of methanol and 300 ml of water were sequentially added. Then, extraction was carried out with ISOPAR-E (hydrocarbon solvent manufactured by Exxonmobil: octane: 60-70%, nonane: 30-40%). The resulting ISOPAR-E solution was concentrated under reduced pressure, recrystallized, and then filtered to obtain acaricidin A 3 and acaricidin A 4 3.06 g of crystals (yield 75%). Its purity is 95% (Acaricidin A 3 : 15.2%; Acaricidin A 4 : 79.8%).

[0044] Acaricidin A 3 and acaricidin A...

reference example 1

[0051] Concentrated acaridin A 3 and acaricidin A 4 1 L of methanol solution prepared from the residue of the fermentation culture broth, and the obtained residue was adsorbed to silica gel (Using Wakol C-100, 400 g) column chromatography. It was developed in ethyl acetate-hexane mixed solution, and the concentrated product contained acaricidin A 3 and acaricidin A 4 fractions. After the obtained residue was recrystallized, 2.69 g of crystals of acaricidin were obtained by filtration (yield 78%). Its purity is 95% (Acaricidin A 3 : 14.3%; Acaricidin A 4 : 80.7%).

[0052] The present invention provides a method for purifying acaricids that does not use chromatography, is simple, economical, and has a high purification effect.

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Abstract

This present invention relates to a method for the purification of milbemycins which comprises washing a milbemycin with a base. According to the method, impurities can be easily removed without using an industrially troublesome technique such as chromatography.

Description

technical field [0001] The invention relates to an industrial-grade refining method of milbemycins. Background technique [0002] Acaricids, which are 16-membered ring macrolide compounds derived from microbial metabolites, are known to have insecticidal, acaricidal and anthelmintic activities, and examples thereof include compounds shown in Table 1 below. [0003] Table 1 [0004] [0005] When such compounds are manufactured, they usually contain a large number of analogs and impurities, as do all microbial metabolites. Therefore, when this type of compound is produced industrially, it must be refined by a method that can be used in industrial production. [0006] As a general purification method of the above-mentioned compound, it is known that the above-mentioned compound is extracted from the fermentation culture with an organic solvent, and then purified by using silica gel, alumina, dextran gel, ion exchange resin, synthetic adsorbent, molecular sieve, C 8 h 1...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 筑山孝弘末本一美佐藤一雄
Owner MITSUI CHEM AGRO INC
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