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
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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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