Azoxystrobin acetone solvate and preparation method thereof

A technology of acetone solvent and solvate, applied in the field of azoxystrobin acetone solvate and preparation, can solve the problems of difficult filtration, high cost, low efficiency, etc., and achieve the effects of not easy to coalesce, complete crystal habit, and low energy consumption

Active Publication Date: 2018-12-07
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The second object of the present invention is to: provide a kind of preparation method of azoxystrobin acetone solvate that is easy to prepare, good in reproducibility, good in fluidity, and suitable for industrial production, and solve the problems of difficult filtration, high cost and low efficiency in production. problems, filling technical gaps

Method used

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  • Azoxystrobin acetone solvate and preparation method thereof
  • Azoxystrobin acetone solvate and preparation method thereof
  • Azoxystrobin acetone solvate and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Take 20g of acetone into the crystallizer, stir at 20°C, add 5g of azoxystrobin raw material into the crystallizer in 2 batches for suspension crystallization, after adding the raw material, continue to stir the solution for 1h, filter the solid, and dry to obtain the product. The X-ray powder diffraction pattern of the product is as follows figure 1 , at 7.32±0.20°, 8.42±0.20°, 13.26±0.20°, 14.16±0.20°, 18.04±0.20°, 18.52±0.20°, 18.90±0.20°, 20.40±0.20°, 21.04±0.20°, 22.36±0.20 °, 23.96±0.20°, 24.36±0.20°, 26.46±0.20°, 28.42±0.20°, 30.06±0.20°, etc. have characteristic peaks, of which 7.32±0.20° is the initial peak, and the relative intensity is 100%. Its TGA results are as follows figure 2 , there will be a weight loss of 13.1%±0.5% before heating to 80°C. Its DSC results are as follows image 3 , there is an endothermic peak at 55.0±5°C, an endothermic and exothermic peak at 104.5±5°C, and a characteristic melting peak at 116.6±5°C. Its IR result is as Figure ...

Embodiment 2

[0040] Take 25g of acetone into the crystallizer, stir at 25°C, add 6g of azoxystrobin raw material into the crystallizer in 3 batches for suspension crystallization, after adding the raw material, continue to stir the solution for 1.5h, filter the solid, and dry to obtain the product. The X-ray powder diffraction pattern of the product is as follows figure 1 . Its TGA and DSC curves are as figure 2 , image 3 . Its infrared spectrum (IR) is as Figure 4 . crystal shape and Figure 5 Similar to a rod. It shows that what is obtained is azoxystrobin acetone solvate. Its volume average particle size is 40μm, its angle of repose is 26°, it does not coalesce and has good fluidity. The XRPD of the azoxystrobin raw material crystal form is as follows: Figure 7 It is Form A.

Embodiment 3

[0042] Add 30g of acetone into the crystallizer, stir at 30°C, add 8g of azoxystrobin raw material into the crystallizer in 2 batches, and carry out suspension crystallization. After adding the raw materials, continue to stir the solution for 2h, filter the solid, and dry to obtain the product. The X-ray powder diffraction pattern of the product is as follows figure 1 . Its TGA and DSC curves are as figure 2 , image 3 . Its infrared spectrum (IR) is as Figure 4 . crystal shape and Figure 5 Similar to a rod. It shows that what is obtained is azoxystrobin acetone solvate. Its volume average particle size is 40μm, its angle of repose is 22°, it does not coalesce and has good fluidity. The XRPD of the azoxystrobin raw material crystal form is as follows: Figure 7 It is Form A.

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Abstract

The invention relates to an azoxystrobin acetone solvate and a preparation method thereof. Characteristic peaks exist at positions with the following diffraction angles represented by 2theta angles: 7.32+ / -0.20 degrees, 8.42+ / -0.20 degrees, 13.26+ / -0.20 degrees, 14.16+ / -0.20 degrees, 18.04+ / -0.20 degrees, 18.52+ / -0.20 degrees, 18.90+ / -0.20 degrees, 20.40+ / -0.20 degrees, 21.04+ / -0.20 degrees, 22.36+ / -0.20 degrees, 23.96+ / -0.20 degrees, 24.36+ / -0.20 degrees, 26.46+ / -0.20 degrees, 28.4+ / -0.20 degrees, 30.06+ / -0.20 degrees and the like, wherein the characteristic peak at the position with the diffraction angle 2theta of 7.32+ / -0.20 degrees is an initial peak, and the relative strength is 100%. The preparation method is a constant-temperature suspension rotating crystal method, operation is simple, control is easy, reproducibility is good, the problems of difficult filtering and low efficiency in production are solved, and the preparation method is suitable for industrialization.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to azoxystrobin acetone solvate and a preparation method. Background technique [0002] The phenomenon of drug solvation exists widely in the process of drug development. Solvates can improve the physical and chemical properties of drugs, promote absorption, and increase the bioavailability of drugs. [0003] Azoxystrobin, the chemical name is 3-(E)-2-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]-phenyl]-3-methoxy base - acrylate, molecular formula: C 22 h 17 N 3 o 5 , its chemical structure is as follows: [0004] [0005] Azoxystrobin is the methoxyacrylate fungicide with the largest sales volume in the world. It is another new type of agricultural fungicide with great development potential and market vitality after triazole fungicides in the pesticide industry. It has good activity against almost all fungal diseases, and can be used in gardening, agri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/52A01N43/54A01P3/00
CPCA01N43/54C07B2200/13C07D239/52
Inventor 龚俊波杨海燕刘裕侯宝红陈明洋贾丽娜
Owner TIANJIN UNIV
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