反应详情

温度

100 °C

A mixture of (S)-1-(1-phenyl-1H-benzoimidazol-2-yl)propylamine from Example 12 (100 mg, 0.398 mmol), 6-chloro-9H-purine (65 mg, 0.418 mmol) and DIPEA (0.348 mL, 2.0 mmol) in dioxane (3 mL) was stirred for 24 h at 100° C. After cooling to RT, volatiles were removed under reduced pressure and the resulting residue was purified by column chromatography (Si—PCC, gradient 0-20% MeOH in EtOAc) and then crystallised from acetonitrile affording 119 as a white solid (50 mg, 34%). LCMS: RT 3.23 min [M+H]+ 370.0. 1H NMR (DMSO, 400 MHz): δ 8.21-8.07 (2H, m), 7.86-7.49 (7H, m), 7.28-7.17 (2H, m), 7.08 (1H, d, J=7.68 Hz), 5.42 (1H, br), 2.08-1.90 (2H, m), 0.83 (3H, t, J=7.32 Hz)

1. temperatureAfter cooling to RT
2. customvolatiles were removed under reduced pressure
3. customthe resulting residue was purified by column chromatography (Si—PCC, gradient 0-20% MeOH in EtOAc)
4. customcrystallised from acetonitrile affording 119 as a white solid (50 mg, 34%)