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Azoxystrobin 1,4-dioxane solvate and preparation method thereof

A technology of dioxane and solvate, applied in the field of azoxystrobin 1, can solve the problems of high cost, low efficiency, difficult filtration, etc., and achieve the effects of easy control, low energy consumption, and uniform particle size distribution

Active Publication Date: 2021-07-13
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The second object of the present invention is to: provide a kind of preparation method of azoxystrobin 1,4-dioxane solvate that is easy to prepare, good in reproducibility, good in fluidity, and suitable for industrial production, so as to solve the difficulties of filtration in production, Problems of high cost and low efficiency, filling the technical gap

Method used

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  • Azoxystrobin 1,4-dioxane solvate and preparation method thereof
  • Azoxystrobin 1,4-dioxane solvate and preparation method thereof
  • Azoxystrobin 1,4-dioxane solvate and preparation method thereof

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Effect test

Embodiment 1

[0038] Take 0.5g of azoxystrobin raw material and place it in a 4mL sample bottle, add 2g of 1,4-dioxane, ultrasonically dissolve it and make it supersaturated, stir in a water bath at 20°C for 1 hour, centrifuge the solution, discard Remove the supernatant and dry the centrifuged solid to obtain the azoxystrobin 1,4-dioxane solvate. The XRPD results are as follows: figure 1 , at 8.40±0.20°, 12.96±0.20°, 14.32±0.20°, 15.20±0.20°, 16.06±0.20°, 17.80±0.20°, 18.62±0.20°, 20.16±0.20°, 21.18±0.20°, 21.56±0.20 °, 22.44±0.20°, 23.76±0.20°, 24.22±0.20°, 25.72±0.20°, 26.32±0.20° have characteristic peaks, of which 8.40±0.20° is the initial peak, and the relative 100% strength. Its TGA results are as follows figure 2 , there will be a weight loss of 16.5%±0.5% before heating to 100°C. Its DSC results are as follows image 3 , there is an endothermic peak at 64.3±5°C, an endothermic and exothermic peak at 103.8±5°C, and a characteristic melting peak at 116.4±5°C. Its IR result is a...

Embodiment 2

[0040] Keep the temperature at 25°C, add 20g of 1,4-dioxane into the crystallizer, and stir to keep the system in a good mixing state. Add 6g of azoxystrobin raw material into the crystallizer, 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 Same as rod. It shows that what is obtained is azoxystrobin 1,4-dioxane solvate. Its volume average particle size is 41μm, 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

[0042] With a constant temperature of 30°C, add 25g of 1,4-dioxane into the crystallizer and stir to keep the system in a good mixing state. Add 8g of azoxystrobin raw material into the finalizer, 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 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 Same as rod. It shows that what is obtained is azoxystrobin 1,4-dioxane solvate. Its volume average particle size is 41μm, its angle of repose is 25°, 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 1,4-dioxane solvate and a preparation method. Its X-ray powder diffraction diffraction angle expressed in 2θ angle is 8.40±0.20°, 12.96±0.20°, 14.32±0.20°, 15.20±0.20°, 16.06±0.20°, 17.80±0.20°, 18.62±0.20°, 20.16 There are characteristic peaks at ±0.20°, 21.18±0.20°, 21.56±0.20°, 22.44±0.20°, 23.76±0.20°, 24.22±0.20°, 25.72±0.20°, 26.32±0.20°, starting from 8.40±0.20° The initial peak, the relative intensity of the characteristic peak at 23.76±0.20° is 100%. The preparation method is simple, the product has high crystallinity, large particle size, good fluidity and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical crystallization, and in particular relates to azoxystrobin 1,4-dioxane 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. 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 an important research content in the process of drug development. [0003] Azoxystrobin, the chemical name is 3-(E)-2-[2-[6-(...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/52
CPCC07B2200/13C07D239/52
Inventor 龚俊波杨海燕刘裕侯宝红贾丽娜吴送姑
Owner TIANJIN UNIV
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