New crystal form of riociguat and preparation method thereof
A crystal form, Leo's technology, applied in the field of medicine, can solve the problems of solvent toxicity and unsuitability for medicinal use, and achieve the effects of stable chemical and physical properties, uniform crystal particles, and convenient manufacturing process
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Embodiment 1
[0022] Take 10g of riociguat and heat it to 70°C with 2 times the volume of DMSO to dissolve it, add 14 times the volume of ethyl acetate, stir at 70°C for 0.5h, then cool to 10°C, stir for 4h, and filter to obtain Cake A; add 14 times the volume of ethyl acetate to filter cake A, heat to reflux, beat for 1 hour, cool to 10°C, stir for 4 hours, and filter to obtain filter cake B; filter cake B is vacuum-dried at 40°C for 18 hours to obtain profit The new crystal form of Ociguat is 4.6g.
Embodiment 2
[0024] Take 10g of riociguat and heat it to 80°C with 2 times the volume of DMSO to dissolve it, add 14 times the volume of ethyl acetate, stir at 80°C for 0.5h, then cool to 15°C, stir for 5h, and filter to obtain Cake A; add 14 times the volume of ethyl acetate to filter cake A, heat to reflux, beat for 1 hour, cool to 15°C, stir for 5 hours, and filter to obtain filter cake B; vacuum-dry filter cake B at 45°C for 20 hours to obtain profit The new crystal form of Ociguat is 4.2g.
Embodiment 3
[0026] Take 10g of riociguat and heat it to 75°C with 2 times the volume of DMSO to dissolve it, add 14 times the volume of ethyl acetate, stir at 75°C for 0.5h, then cool to 12°C, stir for 4.5h, and filter to obtain Filter cake A; add 14 times the volume of ethyl acetate to filter cake A, heat to reflux, beat for 1 hour, cool to 12°C, stir for 4.5 hours, and filter to obtain filter cake B; filter cake B is vacuum-dried at 42°C for 19 hours, Obtained 6.0g of the new crystal form of riociguat.
[0027] The new crystal form of Riociguat obtained by adopting the above-mentioned embodiments 1-3 shows the pattern of the peak shown in the following table in the X-ray powder diffraction pattern in units of 2 θ degrees:
[0028]
[0029] The riociguat crystalline powder obtained in the above-mentioned Example 3 was taken to conduct an investigation experiment on factors affecting stability (including strong light irradiation, high temperature, and high humidity). Among them, the r...
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