FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing a crystalline form of 3-((3S,4R)-3-methyl-6-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1,6-diazaspiro[3.4]octane-1-yl)-3-oxopropane nitrile, having Form β, having a powder X-ray diffraction spectrum containing characteristic peaks with values of 2θ (°): 10.5 ± 0.2, 11.8 ± 0.2, 19.3 ± 0.2 and 22.0 ± 0.2. Method is carried out by crystallisation 3-((3S,4R)-3-methyl-6-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1,6-diazaspiro[3.4]octan-1-yl)-3-oxopropane nitrile from a solvent, in which solvent contains 1:3 (vol./vol.) of 1-butanol and acetonitrile, respectively. Mixture of the compound and the solvent is stirred at 40 °C for 10 days, with subsequent cooling to room temperature.
EFFECT: obtaining a stable crystalline form of 3-((3S,4R)-3-methyl-6-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1,6-diazaspiro[3.4]octan-1-yl)-3-oxopropane nitrile.
1 cl, 17 dwg, 14 tbl, 10 ex
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Authors
Dates
2025-04-24—Published
2017-12-20—Filed