Preparation method for amorphous form of canagliflozin
A canagliflozin and amorphous technology, applied in the field of medicinal chemistry, can solve problems such as high equipment requirements, high industrialization costs, and difficulty in control, and achieve the effects of good fluidity, easy recovery, and low product loss
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Embodiment 1
[0049] Add 20 g of canagliflozin and 60 ml of ethyl acetate into the reaction bottle, stir at a temperature of 35-45°C until it dissolves, and then distill under reduced pressure at a temperature of 35-45°C to a residual weight of 21.0 g to obtain an oily substance. Add 100ml of n-heptane dropwise to the reaction bottle, after the dropwise addition, keep the temperature at 10-20°C for 2 hours. After the heat preservation was completed, the temperature was lowered to 0°C, filtered, and the filter cake was vacuum-dried at 20°C, and discharged to obtain 19.2 g of canagliflozin amorphous as a white powdery solid with a yield of 96.0%. The ethyl acetate recovered by distillation and the n-heptane in the mother liquor can be used directly after simple water removal.
[0050] figure 1 It is the X-ray powder diffraction pattern of the canagliflozin amorphous that embodiment 1 obtains, from figure 1 It can be seen that the diffraction pattern is a typical amorphous substance.
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Embodiment 2
[0055] Add 20 g of canagliflozin and 20 ml of ethyl acetate to the reaction bottle, stir at a temperature of 60-70°C until it dissolves, and then distill under reduced pressure at a temperature of 75-85°C to a residual weight of 21.2g to obtain an oily substance. Add 80 ml of cyclohexane dropwise to the reaction bottle, after the dropwise addition is completed, keep the temperature at 20-30°C for 2 hours. After the heat preservation was completed, the temperature was lowered to 5° C., filtered, and the filter cake was vacuum-dried at 30° C., and discharged to obtain 19.1 g of canagliflozin amorphous as a white powdery solid with a yield of 95.5%.
Embodiment 3
[0057] Add 20 g of canagliflozin and 20 ml of ethanol to the reaction bottle, stir at a temperature of 65-70°C until it dissolves, and then distill under reduced pressure at a temperature of 45-55°C to a residual weight of 22.0g to obtain an oily substance. Add 60 ml of cyclohexane dropwise to the reaction bottle, after the dropwise addition is complete, keep the temperature at 15-25°C for 2 hours. After heat preservation was completed, the temperature was lowered to 10°C, filtered, the filter cake was dried at 30°C, and discharged to obtain 19.4 g of canagliflozin amorphous as a white powdery solid with a yield of 97.0%.
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