FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing a crystalline anhydrous solid form of compound 1, which is form A1, characterized by four or more 2θ RPD peaks at 17.1 ± 0.2°, 17.4 ± 0.2°, 18.8 ± 0.2°, 20.0 ± 0.2° and 21.1 ± 0.2°, which involves dissolving compound 1 in an organic solvent between about 20 °C and 75 °C. Solvents are ethanol, 1-propanol, 2-propanol, 2-butanol, acetone, methyl ethyl ketone, methyl isobutyl ketone, ethyl acetate, 1,4-dioxane, diethyl ether, methyl tert-butyl ether, tetrahydrofuran, acetonitrile, dichloromethane, chloroform, toluene or pyridine, 1-butanol, iso-butanol, N,N-dimethylformamide, ortho-xylene, para-xylene or a mixture thereof, when dissolving compound 1 at 50 °C.
EFFECT: crystalline form of 1-(4-{[6-amino-5-(4-phenoxy-phenyl)-pyrimidin-4-ylamino]-methyl}-4-fluoro-piperidin-1-yl)-propenone (compound 1), having good crystallinity, easy hygroscopicity, high thermal stability.
6 cl, 57 dwg, 7 ex
Title |
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CRYSTALLINE FUMARATE SALT OF (S)-[3,4-DIFLUORO-2-(2-FLUORO-4-IODOPHENYLAMINO)PHENYL][3-HYDROXY-3-(PIPERIDINE-2-YL)AZETIDINE-1-YL]METHANONE |
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