Salt of 2-(substituted pyrimidinyl) thiazole carboxamide compound, as well as composition and use thereof
A compound, p-toluenesulfonate technology, applied in the field of salt or crystal pharmaceutical composition, can solve undisclosed problems
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Embodiment 1
[0162] Example 1 Phosphate Form A1 of the present invention
[0163] 1. Preparation of phosphate crystal form A1
[0164] In a 250mL round-bottomed flask, add free forms of the compound (2.01g) shown in formula (I) and DMF (40mL), stir and dissolve at room temperature, add 1mmol / mL phosphoric acid solution (4.8mL), then add acetone (50mL ), stirring at room temperature for 24h, a large amount of solids were precipitated. After suction filtration, the solid was dried in vacuo to obtain a light yellow solid with a yield of about 85%, which was phosphate crystal form A1.
[0165] 2. Characterization of phosphate crystal form A1
[0166] Identified by Empyrean X-ray powder diffraction (XRPD) analysis: using Cu-Kα radiation, containing the following diffraction peaks expressed in angle 2θ: 5.67°, 7.23°, 11.22°, 12.55°, 13.64°, 14.43°, 16.12°, 17.16 °, 19.71°, 20.49°, 21.35°, 21.96°, 22.94°, 24.56°, 25.45°, 27.69°, 28.41°, there is an error margin of ±0.2°.
[0167] Specific...
Embodiment 2
[0168] Embodiment 2 Phosphate salt crystal form A of the present invention
[0169] 1. Preparation of Phosphate Form A
[0170] In a 250mL round-bottomed flask, add the compound (2.01g) and DMF (40mL) shown in the free form of formula (I), stir and dissolve at room temperature; add 1mmol / mL phosphoric acid solution (4.8mL), then add acetone (50mL ), stirring at room temperature for 24h, a large amount of solids were precipitated. Suction filtration, add purified water (50mL) to the dried solid, heat to 80°C and stir for 8h, suction filtration, vacuum drying to obtain a light yellow solid with a yield of about 85%, which is phosphate crystal form A.
[0171] 2. Characterization of Phosphate Form A
[0172] (1) Analysis and identification by Empyrean X-ray powder diffraction (XRPD): using Cu-Kα radiation, including the following diffraction peaks expressed in angle 2θ: 9.65°, 11.14°, 12.25°, 13.50°, 15.98°, 16.28°, 16.38 °,16.86°,17.20°,19.36°,20.31°,20.79°,20.93°,21.68°,...
Embodiment 3
[0176] Embodiment 3 Phosphate salt crystal form B of the present invention
[0177] 1. Preparation of Phosphate Form B
[0178] The phosphate crystal form A1 (500.50 mg) of the compound of formula (I) and methanol (10 mL) were sequentially added into a 25 mL round bottom flask, and the mixture was suspended and stirred at 50° C. for 24 h. After suction filtration, vacuum drying at 50°C gave a light yellow solid with a yield of about 80%, which was phosphate crystal form B.
[0179] 2. Characterization of Phosphate Form B
[0180] (1) Analysis and identification by Empyrean X-ray powder diffraction (XRPD): using Cu-Kα radiation, including the following diffraction peaks represented by angle 2θ: 8.17°, 10.08°, 12.38°, 14.82°, 16.55°, 17.77°, 19.18 °, 20.52°, 22.36°, 23.67°, 25.89°, 26.39°, 28.13°, 28.91°, there is an error margin of ±0.2°.
[0181] Specifically, the XRPD pattern of the phosphate crystal form B prepared according to the method of Example 3 of the present i...
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