Polymorph
A crystal form and drug technology, applied in the field of polymorphs, can solve problems such as difficult handling
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Embodiment 1
[0063] Example 1 Polymorphic form isolated from methanol (comparative example)
[0064] The hydrated form of compound I (1.00 g) was dried by stripping twice from methanol:chloroform 2:1. It was then dissolved in refluxing methanol (50 mL) and cooled slowly (over several hours) before stirring at ambient temperature. The product was collected by filtration and washed with methanol, then dried under vacuum.
Embodiment 2
[0065] Example 2 Polymorphic Forms of Compounds of the Invention
[0066] Compound I (48.0 g, hydrated form) was stirred in 2-propanol (638 mL) for 2 hours, then heated to 75° C. with stirring at 0.5° C. / min for 110 minutes, then stirred at 75° C. for 2 hours. The slurry was then cooled to 20°C at 0.3°C / min for 183 minutes to 20°C and then stirred at 20°C under nitrogen for 16 hours. The resulting slurry was filtered (glass funnel P3) and the filter cake was washed with 2-propanol (200 mL). The product was dried under vacuum at ambient temperature for 3 days to yield the polymorphic form of Compound 1 of the invention.
Embodiment 3
[0067] Example 3 Differential Scanning Calorimetry
[0068] DSC data were acquired on a Mettler Toledo DSC1 system using standard STARe software. Samples were prepared by manually pressing material into standard 25 microliter aluminum pans and running a standard scan protocol with a temperature ramp of 5 degrees / minute under a 50 mL / minute headspace nitrogen purge flow. The instrument is calibrated with reference standard melting points of indium and tin. Onset, peak and glass transition temperatures were determined graphically with Mettler Toledo STARe software. The results of the analysis of the materials produced in Examples 1 and 2 are in figure 1 and 2 shown in .
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