FIELD: pharmaceuticals.
SUBSTANCE: embodiments of the method of obtaining crystalline of form A of the compound (2S,3R,4R,5S,6R)-2-(7-chloro-6-(4-cyclopropylbenzyl)-2,3-dihydrobenzofuran-4-yl)-6-(hydroxymethyl)tetrahydro-2H-pyran-3,4,5-triol (compound c28) having an X-ray diffraction spectrum that includes peaks at diffraction angles (2θ), equal to 7.0°±0.2°, 14.9°±0.2°, 17.7°±0.2°, 18.8°±0.2°, 20.6°±0.2° 21.8°±0.2° and 23.5°±0.2° in case of irradiation using Cu-Kα radiation source. One of the embodiments of the method includes the following steps: (1) dissolving the crude compound c28 in methanol (5 times the mass of c28) while stirring at room temperature for 30 minutes; (2) adding distilled water (10 times the amount by weight of c28) dropwise to the reaction mixture and then stirring for 30 minutes; (3) additional addition of distilled water dropwise to the resulting suspension (10 times the amount by weight c28); (4) stirring for 1 hour; (5) filtering and washing the resulting precipitate with distilled water and (6) drying the resulting filtrate in a vacuum oven (50°C, 12 hours) to obtain a white crystal of form B.
EFFECT: obtaining the crystalline form of compound c28.
3 cl, 8 dwg, 12 tbl, 13 ex
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Authors
Dates
2024-03-05—Published
2023-03-10—Filed