Eutectic crystal of acetamiprid, and preparation method and application thereof
A technology of acetamiprid and co-crystal, which is applied in the directions of botanical equipment and method, carboxylate preparation, organic chemical method, etc., can solve the problems of low melting point, low water solubility, inconvenient preparation and storage process, etc., and achieves dissolution rate The effect of improving, high water solubility, and maintaining long-term stability without deterioration
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Embodiment 1
[0038] The preparation method of acetamiprid-oxalic acid cocrystal of the present embodiment is implemented according to the following steps:
[0039] The molar ratio is 1:1 and the mixed powder of acetamiprid bulk drug 2.226g and oxalic acid 0.900g is placed in the round bottom flask, and methanol 50mL is added in the round bottom flask, and the solid-liquid ratio of the mixed powder and methanol is 3.126g: 50 mL, heated and stirred in a water bath at 30°C for 2 hours, then filtered, and the filtrate was left to volatilize for 3 days to collect the solid phase to obtain the acetamiprid-oxalic acid co-crystal, a white crystalline powder. Use D8 X-ray diffractometer of German BRUKER company to measure, the test conditions are Cu-Kα target tube voltage 40kV, tube current 10mA, scan speed 2° / min, the PXRD diffraction pattern of the product can be found in figure 1 .
[0040] In this embodiment, the PXRD characteristic diffraction peaks of the acetamiprid-oxalic acid cocrystal ap...
Embodiment 2
[0042] The preparation method of acetamiprid-oxalic acid cocrystal of the present embodiment is implemented according to the following steps:
[0043] The molar ratio is 1:1 and the mixed powder of acetamiprid bulk drug 0.222g and oxalic acid 0.090g is placed in the round-bottomed flask, and methanol 3mL is added in the round-bottomed flask, and the solid-liquid ratio of mixed powder and methanol is 0.312g: 3mL, heated and stirred in a water bath at 50°C for 2h, then filtered, and the filtrate was left to volatilize for 4 days to collect the solid phase to obtain acetamiprid-oxalic acid eutectic, white crystalline powder. Use German BRUKER company D8 type X-ray diffractometer to measure, test condition is that Cu-Kα target tube voltage 40kV, tube current 10mA, scanning speed are 2° / min, and the PXRD diffraction pattern of product is identical with embodiment 1.
Embodiment 3
[0045] The preparation method of acetamiprid-oxalic acid cocrystal of the present embodiment is implemented according to the following steps:
[0046] The molar ratio is 1:1 and the mixed powder of acetamiprid bulk drug 0.222g and oxalic acid 0.090g is placed in the round bottom flask, and ethanol 10mL is added in the round bottom flask, and the solid-liquid ratio of the mixed powder and ethanol is 0.312g: 10 mL, heated and stirred in a water bath at 30°C for 4 hours, then filtered, and the filtrate was left to volatilize for 5 days to collect the solid phase to obtain the acetamiprid-oxalic acid cocrystal, a white crystalline powder. Use German BRUKER company D8 type X-ray diffractometer to measure, test condition is that Cu-Kα target tube voltage 40kV, tube current 10mA, scanning speed are 2° / min, and the PXRD diffraction pattern of product is identical with embodiment 1.
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Abstract
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