Amorphous form or crystalline form of 2-indoline spirocyclic ketone compound or of salt and solvate thereof
A solvate and compound technology, applied in the field of medicinal chemistry, can solve problems affecting drug uniformity, bioavailability, efficacy and safety, solubility, melting point, density, stability, etc., to avoid bioavailability and drug Efficacy changed, preparation method is simple, and the effect of high development value
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Embodiment 1
[0349] Embodiment 1: Preparation of Formula 1 Compound Sulfate Amorphous Form I
[0350] Weigh the compound of formula 1 (100 mg) and add 0.4 mL of isopropanol to dissolve it by ultrasonic, weigh 18 mg of concentrated sulfuric acid (about 1.2 equivalents) and dissolve it in 0.2 mL of isopropanol, add the acid solution to the sample solution, and stir overnight at room temperature After adding 3.0 mL of isopropanol and continuing to stir for 3 days, the system was an emulsion, which could be separated by centrifugation for more than 30 minutes to obtain a solid, which was dried at 50° C. to obtain the amorphous form I of compound sulfate of formula 1.
Embodiment 2
[0351] Embodiment 2: Preparation of Formula 1 Compound Hydrochloride Amorphous Form II
[0352] Weigh the compound of formula 1 (100 mg), add 0.4 mL of acetone to dissolve it by ultrasonic, weigh 18 mg of concentrated hydrochloric acid (about 1.2 equivalents) and dissolve it in 0.2 mL of acetone, add the acid solution to the sample solution, stir overnight at room temperature, the system becomes viscous , adding 3.0 mL of acetone and continuing to stir overnight, centrifuged, and the solid was kept at 50° C. overnight to obtain the amorphous form II of compound hydrochloride of formula 1.
Embodiment 3
[0353] Embodiment 3: Preparation of formula 1 compound hydrochloride crystalline form III
[0354] Weigh the compound of formula 1 (100 mg), add 1.6 mL of ethyl acetate and heat up to 65 ° C to dissolve, weigh 19 mg of concentrated hydrochloric acid (about 1.2 equivalents) and dissolve it in 0.2 mL of ethyl acetate, add the acid solution to the sample solution, Add 2.0 mL of ethyl acetate and keep stirring at 65°C for 10 minutes, then stop heating, naturally lower to room temperature and stir for 2 days, then centrifuge, and dry the solid at 50°C to obtain compound hydrochloride crystal form III of formula 1.
PUM
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