Hydrochloric Acid → HCID 178495893, compound

Participants

Reaction Steps

To a solution of [(R)-1-(6,7-difluoro-1-phenyl-1H-benzoimidazol-2-yl)-2-methoxyethyl]-[9-(tetrahydro-pyran-2-yl)-9H-purin-6-yl]amine (290 mg, 0.57 mmol) in methanol (5 mL) was added HCl in dioxane (0.5 mL, 4M) and the reaction stirred at RT for 30 min. The reaction mixture was concentrated in vacuo and the resultant residue dissolved in EtOAc (10 mL). The solution was washed with sat. aq. NaHCO3 and the product extracted with EtOAc (3×10 mL). The combined organic extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. The resultant residue was triturated with diethyl ether, collected by filtration and dried in vacuo to yield 190 as a white solid (111 mg, 46%). 1H NMR 400 MHz (DMSO-d6): δ 8.13-7.98 (2H, m), 7.89 (1H, br s), 7.74-7.58 (2H, m), 7.59-7.39 (4H, m), 7.29-7.14 (1H, m), 5.47 (1H, br s), 3.87-3.77 (2H, m), 3.11 (3H, s). LCMS (Method K): RT=3.72 min, [M+H]+=422

Provenance & Evidence