POLYMORPH OF 2-[4-[(METHYLAMINO)CARBONYL]-1H-PYRAZOL-1-YL]ADENOSINE

A new polymorph of 2-[4-[(methylamino)carbonyl]-1H-pyrazol-1-yl]adenosine (designated as polymorph E), characterized by an X-ray diffraction pattern of X-RPD showing the following reflections at 2 Theta=5.8°, 12.3°, 15.9°, 17.3°, 20.5°, 22.6°, 23.6°, 27.7°, and 29.2°, and further characterized by DS...

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Hauptverfasser: DVORAKOVA BARBORA, KVAPIL LUBOMIR, HRADIL PAVEL, SLEZAR PETR, GREPL MARTIN
Format: Patent
Sprache:eng
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Zusammenfassung:A new polymorph of 2-[4-[(methylamino)carbonyl]-1H-pyrazol-1-yl]adenosine (designated as polymorph E), characterized by an X-ray diffraction pattern of X-RPD showing the following reflections at 2 Theta=5.8°, 12.3°, 15.9°, 17.3°, 20.5°, 22.6°, 23.6°, 27.7°, and 29.2°, and further characterized by DSC showing marked endotherm in the range of 258 to 264° C., and further characterized by IR spectra, which is prepared by a procedure comprising the following operations: Mixing of 2-[4-[(methylamino)carbonyl]-1H-pyrazol-1-yl]adenosine with a polar aprotic solvent, preferably with dimethylsulfoxide, and heating to form a saturated solution; Cooling of the saturated solution with formation of a turbid solution of 2-[4-[(methylamino)carbonyl]-1H-pyrazol-1-yl]adenosine; Addition of the turbid solution of 2-[4-[(methylamino)carbonyl]-1H-pyrazol-1-yl]adenosine to a protic solvent, preferably methanol, with separation of a gel-like precipitate; Heating of the separated gel-like precipitate in the protic solvent to the boil with formation of a suspension of polymorph E; Cooling of the suspension, isolation and drying of polymorph E.