FIELD: chemistry.
SUBSTANCE: present invention relates to a method of producing a product of an active compound methyl{4,6-diamino-2-[5-fluoro-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]pyrimidine-5-yl}carbamate of formula (I), in crystalline form of modification I, where the X-ray diffraction pattern of the compound of formula (I) in modification I shows peaks maxima for angle of 2 theta at 5.9, 6.9 and 22.7. When implementing method (a), a compound of formula (I) in solid form is dissolved at temperature of 70–80 °C in DMSO or in DMSO in combination with wetting agent ethanol, (b) the dissolved compound of formula (I) is then crystallized from the solution by adding water as an anti-solvent or water in combination with ethanol, where the ratio of water and ethanol added at step a) or b) is 3:1–4:1 or 9:1 wt./wt., and the addition of water or a combination of water with a wetting agent ethanol is carried out at temperature of 60–80 °C and for 20 min-360 min, (c) formed suspension is then cooled to temperature of 20 °C at a cooling rate of 0.003–0.01 K/s, (d) the crystals formed in step b) are then agglomerated to obtain a product of the active compound by adding an agglomeration liquid, wherein the agglomeration liquid is isopropyl acetate, and where, when a wetting agent is added at step a) and/or b), the ratio of the weight of the liquid for agglomeration and the sum of the weight of the compound of formula (I) plus the weight of the wetting agent added at step a) and/or b) is between 0.85 to 1.3 wt./wt.
EFFECT: product of an active compound of formula (I), having improved properties with respect to capacity for extraction, discharge, transportation, sieving and micronization.
5 cl, 9 dwg, 8 tbl, 18 ex
Title |
Year |
Author |
Number |
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