Azoxystrobin acetone solvate and preparation method thereof
A technology for 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
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Embodiment 1
[0038] 20 g of acetone was added to the crystallizer, stirred at 20 ° C, and 5 g of a 5g pyrosyl ester raw material was added to the crystallizer, and the resuscitation was subjected to suspended crystallization. After the raw material was completed, the solution was continued for 1 h, filtered, dried to obtain a product. X-ray powder diffraction diagram of the product 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 °, 18.20 °, 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 a characteristic peak, of which 7.32 ± 0.20 ° is the starting peak, and the relative intensity is 100%. Its TGA results figure 2 13.1% ± 0.5% weight loss before heating to 80 ° C. Its DSC results image 3 The suction peak in 55.0 ± 5 ° C, a heat-insulating peak in 104.5 ± 5 ° C, a characteristic melt peak at 116.6 ± 5 ° C. Its IR results are like Figure 4 At 3106, 3037, 2957, 1752, 17...
Embodiment 2
[0040] The addition of 25 g of acetone was added to the crystallizer, stirred at 25 ° C, and 6 g of the pyrophochan raw material was added to 3 batches, and the suspended crystal was subjected to a resuscitation. After the raw material was completed, the solution was continued for 1.5 h, filtered into the solid, dried to obtain a product. X-ray powder diffraction diagram of the product figure 1 . Its TGA and DSC curve figure 2 , image 3 . Its infrared map (IR) such as Figure 4 . Crystal shape and Figure 5 Similarly to the rod. It is illustrated by acetone acetone solvate. Its average particle diameter is 40 μm, and the rest angle is 26 °, no coalescence, good fluidity. The calcaneus raw material crystal form XRPD is like Figure 7 Crystal form A.
Embodiment 3
[0042] 30 g of acetone was added to the crystallizer, stirred at 30 ° C, 2 batch of 3 batch of 8 g of Aytini ester raw materials, was subjected to suspended crystallization, after the raw material was added, and the solution was continued for 2 h, filtered into the solid, dried to obtain a product. X-ray powder diffraction diagram of the product figure 1 . Its TGA and DSC curve figure 2 , image 3 . Its infrared map (IR) such as Figure 4 . Crystal shape and Figure 5 Similarly to the rod. It is illustrated by acetone acetone solvate. Its average particle diameter is 40 μm, and the ring is 22 °, no coalescence, and good fluidity. The calcaneus raw material crystal form XRPD is like Figure 7 Crystal form A.
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Abstract
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