METHOD OF OBTAINING A CRYSTALLINE MODIFICATION OF FIII 3Β-HYDROXY-5-ANDROSTEN-17-ONE (DEHYDROEPIANDROSTERONE, PRASTERONE, DHEA). Russian patent published in 2024 - IPC C07J15/00 

FIELD: medicine; pharmaceutical industry.

SUBSTANCE: invention relates to a method of obtaining crystalline modification of 3β-hydroxy-5-androsten-17-one (dehydroepiandrasterone, prasterone, DHEA) FIII, which can be used in medicine and the pharmaceutical industry. Crystal modification of FIII 3β-hydroxy-5-androsten-17-one (dehydroepiandrosterone, prasterone, DHEA) is characterized by the following: (a) a set of interplanar distances and their corresponding intensities: 13.301–5.2; 10.568–11.1; 8.155–6.9; 7.487–39.4; 7.327–49.1; 6.748–47.9; 5.973–45.1; 5.669–100; 5.494–13.5; 5.190–93.3; 5.029–21.9; 4.834–15.7; 4.687–90.9; 4.512–15.5; 4.375–9.4; 4.217–16.4; 4.156–18.9; 3.895–12.3; 3.750–6.6; 3.708–7.0; 3.594–13.6; 3.500–6.2; 3.444–8.8; 3.328–5.6; 3.283–7.2; 3.207–8.1; 3.098–6.9; 2.987–4.2; 2.873–5.4; 2.834–5.5; 2.770–7.1; 2.652–3.4; 2.585–3.7; 2.517–5.6; 2.421–4.5; 2.347–3.3; 2.283–5.5, (b) type of crystal lattice — monoclinic, space group P2₁, a = 14.5339(18) , b = 10.3792(14 ), c = 11.8253(14) , β = 111.559(18) °, V = 1659.1(4) ρ_calc = 1.155 g/cm³, Z = 4 (2) C₁₈H₂₈O₂, (c) IR-Fourier spectra in the regions of stretching vibrations O-H (3,413 and 3,369 cm^-1), C=O (1,740 and 1,724 cm^-1) and C-O (1,067 and 1,057 cm^-1) bonds, the area of stretching vibrations of C-H (3,100–2,800 cm^-1) bonds, and in the area of "fingerprints" (1,500–700 cm^-1). A method of obtaining crystal modification of 3β-hydroxy-5-androsten-17-one (dehydroepiandrasterone, prasterone, DHEA) FIII is characterized by the fact that the original substance 3β-hydroxy-5-androsten-17-one is evaporated at a temperature of 60–150°C in vacuum 5÷ 5×10^-4 Torr in a stream of nitrous oxide - N₂O with a flow rate of 1 to 20 ml/min (2.5*10^-3÷ 5.0*10^-2 mol/h) and condense on chilled to 0°C (273 K) - -196° C (77 K) surfaces.

EFFECT: obtaining a phase-pure modification of the crystalline form of FIII 3β-hydroxy-5-androsten-17-one (dehydroepiandrasterone, prasterone, DHEA).

1 cl, 2 tbl, 6 dwg, 13 ex