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Milbemycin A3 oxime crystal form A and preparation method thereof

A crystal form and seed crystal technology, applied in the fields of botanical equipment and methods, organic chemical methods, biocides, etc., can solve the problems of substances without mention of crystal forms, mixtures and so on.

Inactive Publication Date: 2018-01-16
ZHEJIANG HISUN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the crystal form A of Milbey A3 oxime with a single component
At the same time, the A3 / A4 oxime mixture obtained in the prior art does not mention whether it is a substance with a crystal form, and the latest patent CN201410606012.9 does not mention which crystal form the mixture belongs to

Method used

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  • Milbemycin A3 oxime crystal form A and preparation method thereof
  • Milbemycin A3 oxime crystal form A and preparation method thereof
  • Milbemycin A3 oxime crystal form A and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Add 2.0g of wet product of Milbey A3 oxime into 5ml of ethanol, stir and heat to 50°C, and the wet product is completely dissolved. Add the solution to 15ml of water, control the temperature of the mixture at 40°C after the addition, filter to obtain 1.0 g of wet crystals, and dry the crystals in vacuum at 70°C for 48 hours.

[0061] Determined by X-ray powder diffraction, infrared, DSC and TGA, it is confirmed to be Milbey A3 oxime crystal form A, and its X-ray powder diffraction, infrared, DSC and TGA spectra are as follows Figures 1 to 4 shown.

Embodiment 2

[0063] Add 2.0g of Mirbey A3 oxime wet product into 5ml of ethanol, stir and heat to reflux, and the wet product is completely dissolved. Add the solution to 15ml of water, control the temperature of the mixture to 50°C after the addition, filter to obtain 0.8g of wet crystals, and dry the crystals in vacuum at 70°C for 48 hours. After testing, Milbe A3 oxime crystal form A was obtained.

Embodiment 3

[0065] Add 1.5g of wet product of Milbey A3 oxime into 5ml of ethanol, stir and heat to 60°C, and the wet product is completely dissolved. Add the solution to 15ml of water, control the temperature of the mixture at 45°C after the addition, filter to obtain 0.8g of wet crystals, and dry the crystals in vacuum at 70°C for 48 hours. After testing, Milbe A3 oxime crystal form A was obtained.

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Abstract

The present invention relates to the field of pharmaceuticals, especially veterinary medicines, and more particularly relates to a milbemycin A3 oxime crystal form A which can be characterized by X-ray powder diffraction spectroscopy, infrared absorption (IR) spectroscopy, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and the like. Meanwhile, the present invention alsorelates to a preparation method of the milbemycin A3 oxime crystal form A and use of the milbemycin A3 oxime crystal form A as insecticidal acaricides.

Description

technical field [0001] The invention relates to the field of pharmacy, especially the field of veterinary medicine. More specifically, the present invention relates to Milbe A3 oxime crystal form A, a preparation method of the crystal form and the use of the crystal form as an insecticide and acaricide. Background technique [0002] Milbemycin is a microbial natural product pesticide, and existing data show that it is one of the best acaricides in the world today. The U.S. Environmental Protection Agency recognizes it as a low-risk pesticide, and the Netherlands approves it as "GNO" (natural product in crop production). It is an eco-friendly pesticide, suitable for the integrated control of organic agricultural pests and diseases, and has become a popular insecticide and acaricide in developed countries. [0003] Milbemycin is a metabolite with anti-insect activity screened from microbial fermentation broth by Sankyo Company of Japan using Tetranychus urticae as a test ins...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/22A01N43/90A01P7/02A01P7/04
CPCA01N43/90C07D493/22C07B2200/13
Inventor 滕云林慧徐红兵江连清陈正杰白骅
Owner ZHEJIANG HISUN PHARMA CO LTD