Azoxystrobin acetic acid solvate and preparation method thereof

A solvate, azoxystrobin technology, applied in the field of azoxystrobin acetic acid solvate and preparation, can solve the problems of high cost, low efficiency, difficult filtration, etc., and achieve the effect of complete crystal habit, low energy consumption, and improved filtration speed

Active Publication Date: 2021-07-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The second object of the present invention is to: provide a preparation method of azoxystrobin acetic acid 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, Fill technology gaps

Method used

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  • Azoxystrobin acetic acid solvate and preparation method thereof
  • Azoxystrobin acetic acid solvate and preparation method thereof
  • Azoxystrobin acetic acid solvate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Keep the temperature at 20°C, add 20g of acetic acid into the crystallizer, add and stir to keep the system in a good mixing state. Add 5g of azoxystrobin raw material into the crystallizer, after adding the raw material, 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 attached figure 1 , at 7.40±0.20°, 8.28±0.20°, 13.26±0.20°, 14.07±0.20°, 14.52±0.20°, 18.08±0.20°, 18.42±0.20°, 18.86±0.20°, 20.46±0.20°, 21.18±0.20 °, 22.14±0.20°, 22.68±0.20°, 24.46±0.20°, 26.88±0.20°, 28.60±0.20°, etc. have characteristic peaks, 2θ=7.40±0.20° is the initial peak, at 2θ=21.18±0.20° The relative intensity of the characteristic peak at 100%. Its TGA results are as follows figure 2 , there will be a weight loss of 13.0%±0.5% before heating to 100°C. Its DSC results are as follows image 3 , with an endothermic peak at 78.9±5°C and a characteristic melting peak at 110.0±5°C. Its IR result is...

Embodiment 2

[0041] Keep the temperature at 30°C, add 25g of acetic acid into the crystallizer, and stir to keep the system in a good mixing state. Add 6g of azoxystrobin raw material into the finalizer, after adding the raw material, continue to stir the solution for 3h, 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 The same rod shape, smooth surface. It shows that what is obtained is azoxystrobin acetic acid solvate. Its volume average particle size is 36μm, its angle of repose is 24°, 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

[0043] Keep the temperature at 35°C, add 30g of acetic acid into the crystallizer, and stir to keep the system in a good mixing state. Add 10 g of azoxystrobin raw material into the crystallizer, after adding the raw material, continue to stir the solution for 3.5 h, 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 The same rod shape, smooth surface. It shows that what is obtained is azoxystrobin acetic acid solvate. Its volume average particle size is 36μm, 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 azoxystrobin acetic acid solvate and a preparation method thereof. Its X-ray powder diffraction pattern is at diffraction angle 2θ=7.40±0.20°, 8.28±0.20°, 13.26±0.20°, 14.07±0.20°, 14.52±0.20°, 18.08±0.20°, 18.42±0.20°, 18.86±0.20 °, 20.46±0.20°, 21.18±0.20°, 22.14±0.20°, 22.68±0.20°, 24.46±0.20°, 26.88±0.20°, 28.60±0.20°, etc. have characteristic peaks, of which 7.40±0.20° is the starting point peak, the relative intensity of the characteristic peak at 21.18±0.20° is 100%. The preparation method is a constant-temperature suspension crystallization method, and the operation is simple, the reproducibility is good, the product has good fluidity, is not easy to coalesce, and is easy to be industrialized.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to azoxystrobin acetic acid solvate and a preparation method. Background technique [0002] Polymorphism refers to the phenomenon that solid substances form solid states with different physical and chemical properties in two or more different spatial arrangements. In the field of pharmaceutical research, polymorphism includes multi-component crystal forms such as organic solvates and hydrates. [0003] Drug polymorphism widely exists in the drug development process and is an inherent characteristic of small organic molecules. Different crystal forms have different colors, melting points, solubility, dissolution properties, reactivity, chemical stability, mechanical stability, etc. These physical and chemical properties or processability sometimes directly affect the safety and effectiveness of drugs. Therefore, crystal form research and control has become ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/52A01N43/54A01P3/00
CPCA01N43/54C07B2200/13C07D239/52
Inventor 龚俊波杨海燕刘裕侯宝红李鸣晨贾丽娜张诺阳
Owner TIANJIN UNIV
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