反应详情

Alternatively, [(S)-1-(6-Fluoro-1-phenyl-1H-benzoimidazol-2-yl)ethyl]-[9-(tetrahydropyran-2-yl)-9H-purin-6-yl]amine (30 g, 65.6 mmol) was dissolved in EtOAc (200 mL) and HCl (1 M in MeOH, 210 mL) was added dropwise and the resulting solution was stirred for 2 h. The solvents were removed in vacuo and the resulting solid was recrystallised from hot EtOAc/EtOH to give 123 as a white crystalline solid (11 g, 45%). Further product crystallised from the mother liquors. 1H NMR (MeOD-d4, 400 MHz): δ 8.60 (1H, s), 8.53 (1H, s), 7.8 (1H, dd, J 9.8, 4.2 Hz), 7.67 (5H, br s), 7.42 (1H, td, J 9.2, 2.3 Hz), 7.14 (1H, dd, J 7.1, 2.4 Hz), 5.67 (1H, m), 1.87 (3H, d, J=6.9 Hz)

1. customThe solvents were removed in vacuo
2. customthe resulting solid was recrystallised from hot EtOAc/EtOH