FIELD: crystalline forms.
SUBSTANCE: present invention relates to variants of the method for 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) 6.2° ± 0.2°, 7.2° ± 0.2°, 8.8° ± 0.2°, 17.6° ± 0.2°, 19.0° ± 0.2°, 22.5° ± 0.2° and 25.1° ± 0.2° in case of irradiation using Cu-Kα radiation source. One of the variants of the method includes the following steps: (1) dissolving the crude compound c28 in toluene (8 times the mass of c28) by heating at 40°C within 30 minutes; (2) cooling the resulting solution to room temperature to form a suspension; (3) stirring the suspension for 30 minutes; (4) filtering and washing the resulting residue with toluene; and (5) drying in a vacuum oven (50°C, 12 hours) to obtain a white crystal of form A.
EFFECT: obtaining a crystalline form with excellent physical and chemical characteristics.
8 cl, 8 dwg, 10 tbl, 11 ex
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Authors
Dates
2023-06-05—Published
2017-06-15—Filed