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Eprinomectin refining method

A technology of acetamido abamectin and a refining method, which is applied in the field of refining acetamido abamectin, can solve the problems of high solvent residue and low product purity, and achieves the advantages of reducing environmental pollution, improving purity and reducing dosage. Effect

Active Publication Date: 2015-10-28
NORTH CHINA PHARMA GROUP AINO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a kind of refining method of acetaminobamectin, to solve the problems of low product purity and high solvent residue in existing refining methods

Method used

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Examples

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Effect test

Embodiment 1

[0027] Take 100g of acetamidoabamectin primary wet powder, add it to 800ml of mixed solvent A composed of (v / v) 80% n-hexane and 20% ethyl acetate, fully stir, and separate solid and liquid to obtain acetamidoabamectin 98g of mycetin pretreatment powder, then heated and dissolved in 250ml of mixed solvent B composed of (v / v) 30% ethanol, 40% acetone, and 30% water, and added 0.5g of acetamidoabamectin crystals at 70°C Seed, cooling crystallization, solid-liquid separation, obtain acetamidoabamectin secondary wet powder 81g, then add it in the 800ml ether, fully stir, solid-liquid separation, obtain acetamidoabamectin post-treatment powder 78g, At 65° C., vacuum-dried for 5 hours to obtain 57 g of acetamidoabamectin fine powder.

Embodiment 2

[0029] Take 100g of acetamidoabamectin primary wet powder, add it to 700ml of mixed solvent A composed of (v / v) 80% n-hexane and 20% ethyl acetate, fully stir, and separate solid and liquid to obtain acetamidoabamectin 96g of mycetin pretreatment powder, then heated and dissolved in 300ml of mixed solvent B composed of (v / v) 30% ethanol, 40% acetone, and 30% water, and added 0.5g of acetamidoabamectin crystals at 65°C Seed, cooling crystallization, solid-liquid separation, obtain acetamidoabamectin secondary wet powder 78g, then add it in the 700ml ether, fully stir, solid-liquid separation, obtain acetamidoabamectin post-treatment powder 75g, At 65° C., vacuum-dried for 5 hours to obtain 54 g of acetamidoabamectin fine powder.

Embodiment 3

[0031] Take 100g of acetaminobamectin primary wet powder, add it to 900ml of mixed solvent A composed of (v / v) 80% n-hexane and 20% ethyl acetate, fully stir, and separate solid and liquid to obtain acetamidobamectin 92g of mycetin pretreatment powder, then heated and dissolved in 500ml of mixed solvent B composed of (v / v) 30% ethanol, 40% acetone, and 30% water, and added 0.5g of acetamidoabamectin crystals at 75°C Seed, cooling crystallization, solid-liquid separation, obtain acetamidoabamectin secondary wet powder 80g, then add it in 900ml ether, fully stir, solid-liquid separation, obtain acetamidoabamectin post-treatment powder 77g, At 65° C., vacuum-dried for 5 hours to obtain 56 g of acetamidoabamectin fine powder.

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Abstract

The invention provides an eprinomectin refining method. The eprinomectin refining method comprises the following steps: primary eprinomectin wet powder is pre-treated by a solvent A at first; then the obtained product is dissolved in a solvent B; eprinomectin seed crystals are added for crystallization; then a solvent C is adopted for aftertreatment; finally, the obtained product is subjected to vacuum drying to acquire eprinomectin refined powder, wherein the solvent A is a mixed solution of one or more of n-hexane, ethyl acetate and water at any proportion; the solvent B is a mixed solution of two or more of acetone, ethanol and water at any proportion; the solvent C is a mixed solution of one or more of ethyl ether and water at any proportion. The obtained product has the purity of 98% or above, the solvent residue is reduced to be within 200 ppm, the consumption of acetonitrile is greatly reduced, the manufacturing cost is lowered, environmental pollution is reduced, the work environment is greatly improved for workers, and the body health of employees is guaranteed.

Description

technical field [0001] The invention relates to a method for refining macrolide antibiotics, in particular to a method for refining acetamidoabamectin. Background technique [0002] Acetaminobamectin is a macrolide antibiotic developed by Merck Company of the United States in 1996. It has high biological activity and low toxicity (to mammals and aquatic organisms), and is a highly effective, broad-spectrum, and low-residue veterinary antibiotic. The latest generation of anthelmintic drugs are mainly used to control internal and external parasites of livestock (especially lactating livestock), especially for most nematodes and arthropods. The mechanism of action of acetaminobamectin is that the drug binds to the specific receptor of the neuron synapse or neuromuscular synapse in the worm body, stimulates the nerve endings to release the neurotransmitter inhibitor γ-aminobutyric acid and opens the glutamate-controlled Chloride ion channel eventually paralyzes the worm, refuse...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
Inventor 孙耀华李学红杨永军赵少品刘书琴王晓宏胡艳霞董哲周兆彬董雪勇
Owner NORTH CHINA PHARMA GROUP AINO
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