Metastable and stable crystal forms of pyroxasulfone as well as preparation method and application of metastable and stable crystal forms of pyroxasulfone

A technology of metazafen and its stable state, which is applied in the field of pesticides and can solve the problems of difficulty in obtaining a stable titanium single crystal form of metazafen

Pending Publication Date: 2022-03-22
芮城华农生物化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This technology solves problems with traditional methods for producing pure forms of nitroimidazoles called SAIDS because they have different types of molecules that are difficult to separate from each other due to their unique shapes like small beads on an elongated rod made up mostly of carbon atoms. These special structures can cause difficulties when trying to make certain drugs such as SALTIN® which contains this drug substance.

Problems solved by technology

Technological Problem: The technical problem addressed in this patented patent relates to finding new ways to produce metzuzanide that can be applied safely without causing harmful side effects when consumers use these compounds due to their ability to kill germ cells effectively while also being able to prevent resistance diseases like leukemia and breast cancer development. Additionally, the discovery of novel materials called metacarboxes plays important roles in developing pharmaceutical compositions containing metozozanidium salt derivatives.

Method used

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  • Metastable and stable crystal forms of pyroxasulfone as well as preparation method and application of metastable and stable crystal forms of pyroxasulfone
  • Metastable and stable crystal forms of pyroxasulfone as well as preparation method and application of metastable and stable crystal forms of pyroxasulfone
  • Metastable and stable crystal forms of pyroxasulfone as well as preparation method and application of metastable and stable crystal forms of pyroxasulfone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] This example provides a method for preparing the stable crystal form of pyrazazone sulfone, which is characterized in that the method comprises the following steps:

[0058] Add 20g of powdery metazafensulfone in a non-single crystal form to a 250mL three-necked round-bottomed flask filled with 110mL of butanone / (methanol / water) volume ratio = 2.9:(0.7:0.3) compound solvent, and install a reflux tube , stir vigorously with a magnet (800 rpm) at a temperature of 65°C for 20 minutes until the solution is clear, stop heating, naturally cool down to about 25°C, a white solid gradually precipitates, continue to stir at room temperature for 6 hours, filter and crystallize, and obtain 17.8g of white fine needle-shaped crystals, liquid chromatography content 99.0%, yield 89%, its melting point is 134.2°C, and it is a specific crystal form by X-ray powder diffraction method, such as figure 1 Shown, called crystal form A. Its thermogravimetric analysis as Image 6 As shown, its...

Embodiment 2

[0077] This example provides a method for preparing the stable crystal form of pyrazazone sulfone, which is characterized in that the method comprises the following steps:

[0078] Add 22g powdery metazafensulfone of non-single crystal form into a 250mL three-necked round-bottomed flask filled with 110mL butanone / n-heptane (3.2:1) compound solvent, install a reflux tube, and magnetically Stir vigorously (800 rpm) for 30 minutes until the solution is clear, stop heating, cool to room temperature, gradually precipitate a white solid, continue stirring for 8 hours, filter and crystallize to obtain 18.4 g of white fine needle crystals, the liquid chromatography content is 99.1% , the yield is 83%, the crystal form is the same as that in Example 1 through characterization, and it is crystal form A.

[0079] Add 31.9g of the crystal form A of metazafenpyrazole into a 500mL autoclave containing 110mL of tetrahydrofuran / toluene (3:1) compound solvent, replace the air in the autoclave ...

Embodiment 3

[0081] This example provides a method for preparing the stable crystal form of pyrazazone sulfone, which is characterized in that the method comprises the following steps:

[0082] Add 19.8g of powdery metazazol sulfone with non-single crystal form into a 250mL three-necked round-bottomed flask filled with 110mL of chloroform / methanol (1.8:1) compound solvent, install a reflux tube, and magnetically Stir vigorously (800 rpm) for 30 minutes until the solution is clear, stop heating, cool to room temperature, gradually precipitate white solids, continue stirring for 20 hours, filter and crystallize to obtain 17.4 g of white fine needle crystals, liquid chromatography content 99.2% , the yield is 87%, the crystal form is the same as that in Example 1 through characterization, and it is crystal form A.

[0083] Add 30.9g of the A crystal form of metazafenazole into a 500mL autoclave filled with 110mL of chloroform / toluene (1.8:1) compound solvent, replace the air in the autoclave ...

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Abstract

The invention provides pyroxasulfone metastable-state and stable-state crystal forms, a preparation method and application, the preparation method comprises the following steps: step 1, stirring and heating pyroxasulfone in a first compound solvent to completely dissolve solids, cooling and crystallizing, filtering and drying to obtain white fine-needle-shaped crystals, namely the metastable-state fine-needle-shaped crystal form A; and 2, mixing the metastable-state fine-needle-shaped crystal form A and a second compound solvent in a pressure kettle, pressurizing in an inert gas atmosphere, keeping the temperature and pressure, keeping the reaction kettle sealed, reacting, cooling, crystallizing, relieving the pressure, filtering and drying to obtain a semitransparent columnar crystal B, namely the stable-state columnar crystal form B. The invention also discloses a preparation method of the stable-state fine-needle-shaped crystal form B. The stable-state fine-needle-shaped crystal form B is prepared from the metastable-state fine-needle-shaped crystal form A and the stable-state columnar crystal form B. The crystal form B subjected to high-temperature, high-pressure and high-supersaturation-degree treatment is a stable-state crystal form, so that the crystal form B is better in stability, lower in hygroscopicity and convenient to store, and single-dosage-form or compound-dosage-form wettable powder, water dispersible granules and other solid preparations prepared from the crystal form B are good in stability and good in pesticide effect and have very high practical value for industrial production, popularization and application of pyroxasulfone.

Description

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Claims

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Application Information

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Owner 芮城华农生物化学有限公司
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