Apabetalone crystal form and preparation method thereof
A crystal form and crystal technology, which is applied in the field of pharmaceutical crystallization, can solve the problems of affecting drug absorption, not suitable for large-scale industrial production, and slow gas phase diffusion, so as to achieve good solid solubility and improve bioavailability.
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Embodiment 1
[0036] Put 0.06g of Apabetalone raw material in a mixed solvent of 2ml of water and 1,4-dioxane (each 1ml of water and 1,4-dioxane), stir at 30°C for suspension crystallization, filter after 48h, White crystals were obtained and dried at 25°C for 12 hours to obtain the 1,4-dioxane solvent compound of Apabetalone. Take 0.03 g of the obtained 1,4-dioxane solvate solid and heat it in a vacuum drying oven at a heating temperature of 130° C. for 10 minutes to obtain white crystals, namely the crystal form A. The powder X-ray diffraction spectrum of crystal form A product shows that there are characteristic peaks at 7.2, 9.9, 12.6, 13.3, 14.4, 16.9, 19.8, 21.8, 24.1 degrees with diffraction angle 2θ, and figure 1 Consistent, the DSC spectrum has characteristic endothermic peaks at 217, 218 and 232°C respectively, which is consistent with image 3 Consistent, confirm that the obtained product is the Apabetalone crystal form A crystal. The obtained crystal has high crystallinity and...
Embodiment 2
[0038]Put 0.08g of Apabetalone raw material in a mixed solvent of 2ml of water and 1,4-dioxane (each 1ml of water and 1,4-dioxane), stir at 40°C for suspension crystallization, filter after 36h, White crystals were obtained, which were dried at 40°C for 6 hours to obtain the 1,4-dioxane solvent compound of Apabetalone. Take 0.03 g of the obtained 1,4-dioxane solvate solid and heat it in a vacuum drying oven at a heating temperature of 150° C. for 10 minutes to obtain white crystals, namely the crystal form A. The powder X-ray diffraction spectrum of crystal form A product shows that there are characteristic peaks at 7.1, 9.8, 12.5, 13.2, 14.3, 16.8, 19.7, 21.7, 24.0 degrees with diffraction angle 2θ, and figure 1 Consistent, the DSC spectrum has characteristic endothermic peaks at 217, 218 and 232°C respectively, which is consistent with image 3 Consistent, confirm that the obtained product is the Apabetalone crystal form A crystal. The obtained crystal has high crystallini...
Embodiment 3
[0040] Put 0.1g of Apabetalone raw material in a mixed solvent of 2ml of water and 1,4-dioxane (each 1ml of water and 1,4-dioxane), stir at 50°C for suspension crystallization, filter after 24h, White crystals were obtained and dried at 25°C for 24 hours to obtain the 1,4-dioxane solvent compound of Apabetalone. Take 0.03 g of the obtained 1,4-dioxane solvate solid and heat it in a vacuum drying oven at a heating temperature of 130° C. for 30 minutes to obtain white crystals, namely the crystal form A. The powder X-ray diffraction spectrum of crystal form A product shows that there are characteristic peaks at 7.0, 9.7, 12.3, 13.0, 14.1, 16.6, 19.5, 21.5, 23.8 degrees with diffraction angle 2θ, and figure 1 Consistent, the DSC spectrum has characteristic endothermic peaks at 217, 218 and 232°C respectively, which is consistent with image 3 Consistent, confirm that the obtained product is the Apabetalone crystal form A crystal. The obtained crystal has high crystallinity and ...
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