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Method for preparing high-purity moxidectin

A high-purity, pre-purification technology, applied in the direction of organic chemistry, drug combination, anti-infective drugs, etc., can solve the problems of complex process, low reusability, large amount of chromatographic solvent, etc., to achieve easy industrialization and improve product purity Effect

Active Publication Date: 2009-02-25
HISUN PHARMACEUTICAL (HANGZHOU) CO LTD
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  • Abstract
  • Description
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Problems solved by technology

This method can obtain the moxictine of purity more than 90%, but this method process is complicated, needs to operate and control all loaded down with trivial details silica gel chromatography, and this chromatographic solvent consumption is bigger, has no effect on the upper column thing that enters silica gel column High water requirements and low reusability lead to lower yields and higher costs for this chromatography

Method used

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  • Method for preparing high-purity moxidectin

Examples

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example 1

[0019] Example 1: the method for preparing high-purity moxidectin

[0020] 1, the fermented liquid that Streptomyces fermentation produces is through solid-liquid separation, and the nemoctine prepurification liquid 100g that obtains after leaching, purity 15%, flows through macroporous adsorption resin column, resin model HP-20 (40 order, Mitsubishi Chemical, Japan), the packing volume in the column is 10L, after the flow is completed, use the ethanol aqueous solution gradient elution, from 50%-90% (V / V) gradient elution, control the elution flow rate 1-1.5 times the column per hour volume, collect the nemoctine fraction, add 1 / 10 volume of dichloromethane to extract the eluted fraction, and then concentrate to dryness under reduced pressure. The concentrate contains 85g of nimoctine, with a content of 46%.

[0021] 2. The above-mentioned nimoctine concentrate was subjected to the upper protection reaction (conventional reaction) to obtain 80 g of the upper protection produc...

example 2

[0024] Example 2: the method for preparing high-purity moxidectin

[0025] 1. The fermented liquid produced by Streptomyces fermentation is subjected to solid-liquid separation, and the pre-purified liquid obtained after leaching has a purity of 18%, and 120g of nimoctine 1.2% (W / W) in the solid, flows through macropores for adsorption Resin column, resin model XAD-1600 (40 mesh, produced by Rohm-Haas Company, the U.S.), the filling volume in the column is 12L, and after the flow is finished, use acetone aqueous solution gradient elution instead, from 50%-80% (V / V) Gradient elution, control the elution flow rate of 1-1.5 times the column volume per hour, collect the nemoctine fraction, add 1 / 10 volume of dichloromethane to the elution fraction for extraction, and concentrate to dryness under reduced pressure. The concentrate contains 98g of nimoctine, with a content of 43.6%.

[0026] 2. The above-mentioned nimoctine concentrate was subjected to the upper protection reaction...

example 3

[0029] Example 3: the method for preparing high-purity moxidectin

[0030] 1. The fermented liquid produced by Streptomyces fermentation is subjected to solid-liquid separation, and the pre-purified liquid obtained after leaching has a purity of 13.8%, and contains 0.8% (W / W) 80.6g of nemoctine in the solid, and flows through the large pores Adsorption resin column, resin type HP-20 (40 mesh, Mitsubishi Chemical, Japan), the volume of the column filling is 10L, after the flow is completed, use 85% ethanol solution to elute, and control the elution flow rate to 1-1.5 times the column per hour volume, collect the nemoctine fraction, add 1 / 10 volume of dichloromethane to extract the eluted fraction, and then concentrate to dryness under reduced pressure. The concentrate contains 68.2 g of nimoctine, with a content of 41.5%.

[0031] 2. The above-mentioned nimoctine concentrate was subjected to the upper protection reaction to obtain 63.8g of the upper protection product, which f...

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Abstract

The invention relates to a method for preparing high-purity Moxidectin, which comprises the following steps: (1) macroporous absorption resin chromatography is carried out on Moxidectin solution which is purified in advance, the obtained product is eluted by the mixed solution of polar organic solvent and water; (2) the eluent is extracted by methylene dichloride, and then solvent is removed by conventional concentration; (3) protective reaction is carried out on the condensate to obtain upper protective liquid; (4) macroporous absorption resin chromatography is carried out on the upper protective liquid, and the chromatography is eluted by the mixed solution of the polar organic solvent and the water; (5) the eluted upper protective liquid is oxidized, and then deprotection and oximation reaction are carried out to obtain the reaction liquid of the Moxidectin; (6) macroporous absorption resin chromatography is carried out on the reaction liquid of the Moxidectin, and the chromatography is eluted by the mixed solution of the polar organic solvent and the water, so that the obtained eluent is the high-purity Moxidectin solution; the product can be separated out of the solution by using the conventional concentration and crystallization technology if necessary. As the macroporous absorption resin chromatography is used for separating instead of silica gel chromatography, the method is not only stable and controllable as well as is easy to industrialize, but also improves the product purity, the quality and the yield.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular, the invention relates to a method for preparing high-purity moxictine. Background technique [0002] The invention relates to a method for preparing moxictine. Moxidectin (INN: Moxidectin) is a macrolide agricultural antibiotic, mainly used to treat parasitic diseases in animals such as cattle and sheep, and can be fermented by Streptomyces to produce Nemodectin (INN: Nemadectin) , and then obtained by chemical reaction. U.S. Patent No. 4,916,154A (its entire content is hereby incorporated as a reference) provides a method for preparing moxictine, that is, the fermented liquid produced after the fermentation of Streptomyces is separated from solid and liquid, and the nemoxictine solution obtained after leaching is passed through Extraction, silica gel column chromatography, gel chromatography to obtain nimoctine with a purity of more than 90% (HPLC), the purified nimoctine is p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/22A61P33/00
Inventor 缪建玉
Owner HISUN PHARMACEUTICAL (HANGZHOU) CO LTD
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