Crystal form of nitrogen-containing tricyclic compound and use thereof
A technology for compounds and crystal forms, applied in the field of pharmaceutical compositions of crystal forms, can solve the problems of undisclosed compound microstructure, undisclosed crystal structure and the like
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Embodiment 1
[0105] Embodiment 1 The crystal form B of the compound of formula (I)
[0106] 1. Preparation of Form B
[0107] Compound 2-((5-cyclopropyl-3-(2,6-dichlorophenyl)isoxazol-4-yl)methoxy)-10H-spiro[benzo[6,7] Oxazo[3,2-b]pyridine-11,1'-cyclopropane]-7-carboxylic acid (223.6 mg) was added to a one-necked bottle, suspended in dimethyl sulfoxide (1.1 mL) and ethyl acetate at room temperature (1.1mL) in a mixed solvent, stirred for 12 hours, then cooled to 6°C, added isopropanol (3.0mL), stirred and crystallized at 6°C for 48 hours, suction filtered, and the filter cake was washed with isopropanol (1.0mL) , dried under vacuum at 80°C for 6 hours to give a white solid (182.1 mg, 81.4%).
[0108] 2. Identification of Form B
[0109] (1) Analysis and identification by Empyrean X-ray powder diffraction (XRPD): using Cu-Kα radiation, it has the following characteristic peaks expressed in angle 2θ: 6.24°, 8.11°, 10.82°, 11.13°, 11.84°, 12.21°, 12.54 °,13.67°,14.02°,14.50°,14.81°,15...
Embodiment 2
[0111] Embodiment 2 The crystal form C of the compound of formula (I)
[0112] 1. Preparation of Form C
[0113] Compound 2-((5-cyclopropyl-3-(2,6-dichlorophenyl)isoxazol-4-yl)methoxy)-10H-spiro[benzo[6,7] Oxazo[3,2-b]pyridine-11,1'-cyclopropane]-7-carboxylic acid (101.3mg) was dissolved in N,N-dimethylacetamide (0.5mL), and the above solution was added dropwise Pour into water (1.0 mL), stir while adding dropwise, continue to stir and crystallize at room temperature for 12 hours after dropping; filter with suction, and dry the filter cake under vacuum at 60°C for 12 hours to obtain a white solid (76.8 mg, 75.8%).
[0114] 2. Identification of Form C
[0115] (1) Analysis and identification by Empyrean X-ray powder diffraction (XRPD): using Cu-Kα radiation, it has the following characteristic peaks expressed in angle 2θ: 7.43°, 8.10°, 10.24°, 10.97°, 11.69°, 12.15°, 13.14 °,13.66°,15.19°,15.46°,16.42°,17.45°,18.06°,18.58°,19.22°,19.66°,20.88°,21.33°,22.01°,22.48°,22.81°...
Embodiment 3
[0117] Embodiment 3 The crystal form E of the compound of formula (I)
[0118] 1. Preparation of Form E
[0119] Compound 2-((5-cyclopropyl-3-(2,6-dichlorophenyl)isoxazol-4-yl)methoxy)-10H-spiro[benzo[6,7] Oxazo[3,2-b]pyridine-11,1'-cyclopropane]-7-carboxylic acid (199.6mg) was added to a one-necked bottle, dissolved in acetone (3.0mL) at room temperature, cooled to -10°C, Stir and crystallize for 12 hours; filter with suction, and dry the filter cake under vacuum at room temperature for 4 hours to obtain a white solid (96.2 mg, 48.2%).
[0120] 2. Identification of Form E
[0121] (1) Analysis and identification by Empyrean X-ray powder diffraction (XRPD): using Cu-Kα radiation, it has the following characteristic peaks expressed in angle 2θ: 6.23°, 7.08°, 8.12°, 10.97°, 12.50°, 13.88°, 14.23 °,15.77°,16.18°,17.20°,18.15°,18.65°,18.81°,20.31°,20.88°,21.49°,21.77°,22.05°,22.21°,22.49°,22.74°,23.19°,24.16°, 24.48°,24.7°,25.20°,25.39°,25.98°,26.19°,26.67°,27.50°,28.20°,2...
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