Phosphate of 2-(substituted pyrimidinyl) thiazole carboxamide compound and use of phosphate
A phosphate and compound technology, applied in the field of medicine, can solve undisclosed problems
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
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 aqueous 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°. Specifical...
Embodiment 2
[0167] Embodiment 2 Phosphate salt crystal form D of the present invention
[0168] 1. Preparation of Phosphate Form D
[0169] Phosphate crystal form A1 (502.50mg) and N,N-dimethylacetamide (5mL) of the compound represented by formula (I) were sequentially added into a 25mL round bottom flask, suspended and stirred at 50°C for 24h. After suction filtration, vacuum drying at 50°C gave a light yellow solid with a yield of about 88%, which was phosphate crystal form D.
[0170] 2. Characterization of Phosphate Form D
[0171] (1) Analysis and identification by Empyrean X-ray powder diffraction (XRPD): using Cu-Kα radiation, including the following diffraction peaks represented by angle 2θ: 5.54°, 11.17°, 13.41°, 15.61°, 16.06°, 16.73°, 18.28 °,18.96°,19.80°,20.14°,20.96°,22.05°,22.39°,22.67°,24.13°,25.13°,26.09°,26.84°,27.34°,28.20°,28.57°,30.49°,31.73°, 32.65°, there is an error margin of ±0.2°. Specifically, the XRPD pattern of the phosphate crystal form D prepared acc...
Embodiment 3
[0173] Embodiment 3 Phosphate Form F of the present invention
[0174] 1. Preparation of Phosphate Form F
[0175] Add the phosphate crystal form A1 (100.50mg) and DMF (3mL) of the compound of formula (I) into a round bottom flask, stir and dissolve at room temperature, and spin evaporate under reduced pressure at 60°C to obtain a light yellow solid with a yield of about 88%. , is phosphate crystal form F.
[0176] 2. Characterization of Phosphate Form F
[0177] (1) Analysis and identification by Empyrean X-ray powder diffraction (XRPD): using Cu-Kα radiation, including the following diffraction peaks expressed in angle 2θ: 5.55°, 10.26°, 11.21°, 12.39°, 13.56°, 14.21°, 16.09 °, 16.80°, 18.39°, 19.02°, 19.15°, 20.09°, 20.35°, 21.26°, 22.71°, 23.01°, 24.43°, 25.52°, 26.33°, 26.93°, 28.27°, 30.67°, exist ±0.2 ° margin of error. Specifically, the XRPD pattern of the phosphate crystal form F prepared according to the method of Example 3 of the present invention is basical...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More