Crystal forms of octahydropyrrolo[3,4-c]pyrrole derivatives
A crystal form and drug technology, which can be used in drug combinations, medical preparations containing active ingredients, allergic diseases, etc., and can solve the problems of poor drugability, poor water solubility, and low oral bioavailability.
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Embodiment 1
[0128] Embodiment 1 Crystal form I of the present invention
[0129] 1. Preparation of Form I
[0130] The compound represented by formula (I) (307 g) was prepared with reference to the method of Example 3 in International Application WO 2017088759 A1, which was dissolved in DMF (614 mL), heated to 80° C. and stirred for 0.5 h to dissolve, and then slowly cooled to room temperature , crystallization, suction filtration, the filter residue was washed with water (50 mL × 2), and air-dried at 70°C to obtain an off-white solid powder.
[0131] 2. Identification of Form I
[0132] (1) Identification by Empyrean X-ray powder diffraction (XRPD) analysis: using Cu-Kα radiation, with the following characteristic peaks represented by the angle 2θ: 7.44°, 7.78°, 8.24°, 12.69°, 12.95°, 14.08°, 14.75 °,15.03°,17.75°,19.71°,20.12°,20.81°,21.30°,21.89°,22.18°,23.27°,25.49°,25.85°,26.08°,26.60°,27.21°,27.44°,27.70°, 28.53° with an error tolerance of ±0.2°.
[0133] (2) Identification ...
Embodiment 2
[0134] Example 2 Amorphous of the present invention
[0135] 1. Amorphous Preparation
[0136] The crystalline form I (500 mg) of the compound represented by the formula (I) was added to DCM (5.0 mL), dissolved at room temperature, followed by rotary evaporation under reduced pressure to precipitate a solid, which was dried to obtain an off-white solid powder.
[0137] 2. Identification of Amorphous
[0138] Identified by Empyrean X-ray Powder Diffraction (XRPD) analysis: using Cu-Kα radiation, with substantially as image 3 An X-ray powder diffraction (XRPD) pattern is shown.
Embodiment 3
[0139] Example 3 Crystal form II of the present invention
[0140] 1. Preparation of Form II
[0141] The crystal form I (200 mg) of the compound represented by the formula (I) was added to ethyl acetate (2.0 mL), heated to 75° C. under stirring for 24 h, and the reaction was stopped, suction filtration, and drying to obtain an off-white solid powder, the target crystal form.
[0142] 2. Identification of Form II
[0143] (1) Identification by Empyrean X-ray Powder Diffraction (XRPD) analysis: using Cu-Kα radiation, with the following characteristic peaks represented by angle 2θ: 10.43°, 12.31°, 13.08°, 14.49°, 15.18°, 15.92°, 16.00 °,16.61°,16.90°,17.90°,18.42°,20.52°,21.04°,21.45°,23.59°,24.00°,24.26°,24.75°,25.07°,26.26°,26.53°,26.83°,28.02°, 28.31°, 29.31°, 30.03°, 30.42°, 31.20°, 31.56°, 32.25°, 32.80°, 33.63°, 34.24°, 35.54°, 36.41°, 36.96°, 38.33°, 38.78°, with ±0.2° Error tolerance.
[0144] (2) Identification by TA Q2000 Differential Scanning Calorimetry (DSC...
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