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Method used for preparing moxidectin using nemadectin fermentation broth

A technology of nimoctine formamide and nimoctine dichloromethane, which is applied in the field of preparing moxictine from fermented liquid of nimoctine, and can solve the problems of low yield, high total cost, long analysis time, etc. , to achieve the effect of high total yield, low cost and simple operation

Inactive Publication Date: 2014-03-26
HEBEI YUZE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses three times of resin chromatography. As we all know, the analysis time is long and the yield is low during chromatography, resulting in higher total cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of method that prepares moxictine with fermented liquid of nimoctine, comprises the steps:

[0030] (1) Vacuum filter 26L of nimoctine fermented liquid to separate the solid and liquid to obtain a filter cake (mycelia), then add 15L of ethanol to soak the filter cake to obtain the nimoctine ethanol soaking solution, which is obtained after concentration and removal of ethanol The concentrate of the ethanol soaking solution of nimoctine, which contains 38g of nimoctine, with a purity of 15%.

[0031] (2) Add n-hexane to the concentrate of the above-mentioned nimoctine ethanol soaking solution and stir and extract, the volume of n-hexane used in milliliters is 5 times the concentration of the nimoctine ethanol soaking solution in grams, to obtain nemoctine N-hexane extract was concentrated under reduced pressure to remove n-hexane to obtain the concentrate of nimoctine n-hexane extract, which contained 36g of nimoctine and a purity of 56%.

[0032] (3) Adding form...

Embodiment 2

[0037] A kind of method that prepares moxictine with fermented liquid of nimoctine, comprises the steps:

[0038] (1) Vacuum filter 30L of the fermented nimoctine liquid to obtain a filter cake (mycelium), then add 18L of ethanol to soak to obtain the ethanol soaking liquid of nimoctine, concentrate and remove the ethanol to obtain the nemoctine The concentrate of cretin ethanol soaking solution, which contains 40g of nimoctine, with a purity of 15%.

[0039] (2) Add n-heptane to the concentrate of the above-mentioned nimoctine ethanol soaking solution and stir and extract, and the milliliters of the volume of n-heptane used is 10 times the concentrate grams of the nimoctine ethanol soaking solution to obtain nimoctine The n-heptane extract of moctin was concentrated under reduced pressure to remove the n-heptane to obtain the concentrate of the n-heptane extract of nimoctine, which contained 37g of nimoctine and had a purity of 58%.

[0040] (3) adding formamide to the conce...

Embodiment 3

[0045] A kind of method that prepares moxictine with fermented liquid of nimoctine, comprises the steps:

[0046] (1) Vacuum filtration of 27L of fermented nimoctine to obtain a filter cake (mycelia) after solid-liquid separation, and then soak in 16L of ethanol to obtain a nimoctine ethanol soaking solution, which is then concentrated to remove ethanol to obtain nemoctine The concentrate of cretin ethanol soaking solution, which contains 40g of nimoctine, with a purity of 15%.

[0047] (2) Add sherwood oil to the concentrate of the above-mentioned nimoctine ethanol soaking solution and stir and extract, the milliliters of the volume of sherwood oil used is 8 times the gram number of the concentrate of the nimoctine ethanol soaking solution, to obtain nemoctine The petroleum ether extract of nimoctine was concentrated under reduced pressure to remove the petroleum ether to obtain the concentrate of the petroleum ether extract of nimoctine, which contained 38g of nimoctine and ...

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PUM

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Abstract

The invention discloses a method used for preparing moxidectin using nemadectin fermentation broth, and belongs to the synthesis technology field of compounds with condensed rings containing 4 or more heterocyclic rings. The method comprises following steps: the nemadectin fermentation broth is subjected to solid-liquid separation so as to obtain mycelium; the mycelium is immersed in ethanol so as to obtain an ethanol immersion liquid; the ethanol immersion liquid is condensed, an organic solvent with low polarity is added for extraction, and an obtained product is condensed; methanamide or a mixed solvent of methanamide and a polar solvent is added for extraction so as to obtain an extract liquor; dichloromethane is added for extraction, and an obtained mixture is condensed, and is subjected to chromatography using macroporous resin or silicagel column so as to obtain nemadectin with a purity of more than 85%; and nemadectin is subjected to upper protection, oxidation, oximation, crystallization, deprotection, and chromatography using macroporous resin or silicagel column so as to obtain moxidectin with a purity of more than 93%. The method processes advantages such as short operation time, simple operation, high overall yield, and low cost.

Description

technical field [0001] The invention relates to the technical field of synthesis of compounds containing 4 or more heterocycles in a condensed ring system. Background technique [0002] Moxidectin, also known as Moxidectin (MXD), CAS No. 113507-06-5, is a semi-synthetic single-component macrolide produced by the fermentation of Streptomyces.cyanneogrisens noncyanogenus Antibiotics are derivatives of Nemadectin. [0003] The difference between moxictine and other macrolide antiparasitic drugs ivermectin (Ivermetin, IVM) and avermectin (Avermectin, AVM) is that it is a single component and has a wider repellent effect. Anthelmintic activity and long-acting, safe and other characteristics, and there is a strong anti-nematode and arthropod and other internal and external parasite activity at very low doses. It was only used as an anthelmintic for animals in the mid-1980s, and it is now available in Japan. commoditized. [0004] Chinese Patent Authorization Announcement No. CN...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 杨玉淮赵少欣王建秋韩烁
Owner HEBEI YUZE CHEM TECH
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