Prasugrel hydrochloride ethanol solvate and preparation method thereof
A technology of prasugrel hydrochloride and hydrochloride ethanol, applied in organic chemistry, drug combination, blood diseases, etc., can solve the problems of difficult filtration, viscous crystal slurry, small crystal size, etc., and achieve crystal surface smoothness and product quality The effect of large particle size and efficiency improvement
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Embodiment 1
[0027] Dissolve 3g of prasugrel in 20ml of sec-butanol, add 0.74ml of 12mol / L concentrated hydrochloric acid dropwise under stirring at room temperature, stir for 1h, filter the precipitated crystals, and dissolve the filtered crystals in 10ml of absolute ethanol at 70°C , the initial concentration of the solution was 0.3g / ml, the temperature was lowered to -10°C, the precipitated crystals were filtered, and dried at a vacuum of 0.08MPa and 60°C for 8h to obtain 1.76g of white crystalline prasugrel hydrochloride ethanol solvate. The product has high crystallinity, large crystal size and smooth surface.
[0028] The powder X-ray diffraction pattern of the product is as figure 1 As shown, there are characteristic peaks at diffraction angles (2θ) of 8.22, 11.48, 12.16, 13.00, 13.69, 14.32, 15.96, 17.38, 18.54, 21.70, 23.56, 24.34, 24.98, 26.38 and 28.66 degrees. Infrared spectrum picture as figure 2 Shown at 475, 589, 658, 772, 884, 958, 1035, 1082, 1123, 1287, 1379, 1495, 159...
Embodiment 2
[0030] Dissolve 3g of prasugrel in 25ml of isopropanol, add 0.54ml of 12mol / L concentrated hydrochloric acid dropwise under stirring at room temperature, stir for 1h, filter the precipitated crystals, and dissolve the filtered crystals in 10ml of absolute ethanol at 50°C , the initial concentration of the solution was 0.3g / ml, the temperature was lowered to -5°C, the precipitated crystals were filtered, and dried at 40°C at a vacuum of 0.09MPa for 3h to obtain 1.74g of white crystal prasugrel hydrochloride ethanol solvate. The product has high crystallinity, large crystal size and smooth surface.
[0031] The XRD pattern of the product shows that there are characteristic peaks at diffraction angles (2θ) of 8.23, 11.49, 12.26, 13.12, 13.69, 14.35, 15.98, 17.48, 18.56, 21.75, 23.59, 24.40, 24.99, 26.39 and 28.65 degrees. The infrared spectrum shows that at 475, 507, 589, 658, 668, 693, 735, 771, 813, 8432, 883, 923, 957, 1005, 1035, 1081, 1095, 1123, 1208, 1286, 1326, 1379, 142...
Embodiment 3
[0033]Dissolve 2 g of prasugrel in 15 ml of tetrahydrofuran, add 0.49 ml of 12 mol / L concentrated hydrochloric acid dropwise under stirring at room temperature, stir for 1 h, filter the precipitated crystals, and dissolve the filtered crystals in 10 ml of absolute ethanol at 60°C, and the solution The initial concentration of prasugrel was 0.2g / ml, the temperature was lowered to 0°C, the precipitated crystals were filtered, and dried at a vacuum of 0.1MPa and 50°C for 5h to obtain 1.48g of white crystalline prasugrel hydrochloride ethanol solvate. The product has high crystallinity, large crystal size and smooth surface.
[0034] The XRD pattern of the product shows that there are characteristic peaks at diffraction angles (2θ) of 8.23, 11.49, 12.27, 13.10, 13.68, 14.36, 15.98, 17.48, 18.59, 21.77, 23.50, 24.35, 24.97, 26.38 and 28.66 degrees. The infrared spectrum shows that at 475, 507, 589, 658, 668, 693, 735, 771, 813, 8432, 883, 923, 957, 1005, 1035, 1081, 1095, 1123, 120...
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