Crystals of pon·HCl suitable for analysis by single-crystal X-ray diffraction (SCXRD) were grown in an unconventional manner. Ponatinib freebase was added to a 4 mL vial, and acetonitrile was added on top of the solid material until covered. 1 mL of a solution prepared from acetonitrile (10 mL), formic acid (0.7 mL), water (0.8 mL), and hydrochloric acid (concentrated, 0.2 mL) was then layered over the first acetonitrile solution in the vial. After two days at RT, both white needle and yellow block crystals were seen in the vial. The crystals were carefully separated using the Pasteur method, and PXRD data were acquired for each type of crystal. The yellow block crystals were found to be pon·HCl , and the white needles were found to be the previously reported ponatinib monohydrochloride.69,70
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Crystallization of Ponatinib Hydrochloride
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Other organizations : Apotex Pharmachem (Canada), Florida State University, National High Magnetic Field Laboratory, McMaster University
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Variable analysis
independent variables
- Addition of ponatinib freebase to a 4 mL vial
- Addition of acetonitrile on top of the solid material until covered
- Layering a solution prepared from acetonitrile (10 mL), formic acid (0.7 mL), water (0.8 mL), and hydrochloric acid (concentrated, 0.2 mL) over the first acetonitrile solution in the vial
- Formation of white needle and yellow block crystals in the vial
- Crystal type (yellow block crystals were found to be pon·HCl, and the white needles were found to be the previously reported ponatinib monohydrochloride)
- Reaction time (two days at RT)
- Vial size (4 mL)
- No positive or negative controls were explicitly mentioned in the provided information.
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