Hydrochloric Acid → HCID 178478962, compound

Participants

Reaction Steps

4 Charge 4-{4-[4-(3-Trifluoromethyl-phenyl)-1H-imidazol-2-yl]-piperidin-1-yl}-1H-pyrazolo[3,4-d]pyrimidine (442.9 g, 1.07 mol) along with IPA (4.43 L) and stir the resulting slurry at RT. Slowly add HCl (214 mL of a 5M aqueous solution, 1.07 mol, 1.0 eq) and heat to 50° C. Stir for 30 minutes and add acetone (4.43 L) and continue heating for 4 h. Cool to 15° C. for 2 hr then filter the solid. Wash the filter cake with acetone (800 mL) and dry resulting solid in vacuum oven at 60° C. for 3 h to afford the title compound (458 g, 94%) as a tan to off-white solid. M.p.=306° C.; MS (ES): m/z=414 [M+H]

Provenance & Evidence