FIELD: chemical industry.
SUBSTANCE: invention relates to a method for obtaining a crystalline form ((S)-2,2-difluorocyclopropyl)((1R,5S)-3-(2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)-3,8-diazabicyclo[3.2.1]octan-8-yl)-methanone (Form 1), which is characterized by an x-ray powder diffraction pattern including peaks expressed in angles 2θ, at 5.0, 9.4, 9.9, 14.8, 16.8 and 18.7° 2θ± 0.2° 2θ, where the method includes the introduction of ((S)-2,2-difluorocyclopropyl)-((1R,5S)-3-(2-((1-methyl-1H-pyrazol-4-yl)amino)-pyrimidin-4-yl)-3,8-diazabicyclo[3.2.1]octan-8-yl)methanone into ethanol/water and heating to form a solution followed by cooling to form crystals. The invention also relates to a method for obtaining a crystalline form of ((S)-2,2-difluorocyclopropyl)((1R,5S)-3-(2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4 -yl)-3,8-diazabicyclo[3.2.1]octan-8-yl)-methanone (Form 1), which is characterized by an X-ray powder diffraction pattern including peaks expressed in angles 2θ at 5.0, 9.4, 9.9, 14.8, 16.8 and 18.7° 2θ±0.2° 2θ, where the method includes the introduction of a free base ((S)-2,2-difluorocyclopropyl)-((1R,5S)-3-(2-((1-methyl-1H-pyrazol-4-yl)amino)-pyrimidin- 4-yl)-3,8-diazabicyclo[3.2.1]octan-8-yl)methanone to methylisobutylketone and heating, followed by the addition of n-heptane to form a solution, seeding the solution by introducing a free base ((S)-2,2-difluorocyclopropyl)-((1R,5S)-3-(2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)-3,8-diazabicyclo[3.2.1]octane- 8-yl)methanone followed by cooling to ambient temperature to form crystals.
EFFECT: obtaining a crystalline form of ((S)-2,2-difluorocyclopropyl)((1R,5S)-3-(2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)-3,8-diazabicyclo[3.2.1]octan-8-yl)-methanone.
8 cl, 4 dwg, 4 tbl, 4 ex
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