p-Toluenesulfonate → p-Toluenesulfonic acid monohydrate

Temperature

25 °C

An aliquot (1.5 g, 2.2 mmol) of the tosylate anhydrous form 1 salt form of the compound of Formula I prepared above was dissolved in 4.5 mL of methanol. The solution was concentrated to dryness after 3 days by vacuum distillation. The solids were slurried in 4.5 mL of 2-propanol which was shaken at 25° C. and 350 RPM for six days yielding precipitate. The solids were collected by vacuum filtration and dried under vacuum at room temperature over a 12 hour period. The resulting crystalline tosylate hydrate form 2 salt form of the compound of Formula I was analyzed by X-ray crystallography (FIG. 21), DSC (FIG. 22), and TGA (FIG. 23) in accordance with the procedures described above.

1. concentrationThe solution was concentrated to dryness after 3 days by vacuum distillation
2. custom350 RPM for six days yielding precipitate
3. filtrationThe solids were collected by vacuum filtration
4. customdried under vacuum at room temperature over a 12 hour period

ORD record

ord-55ae6d00d33d4d0fb7789440b769612f

Source dataset

uspto-grants-2011_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07956189B2