反应详情

温度

100 °C

(S)-1-(6-Fluoro-1-isopropyl-1H-benzoimidazol-2-yl)ethylamine (0.5 g, 2.26 mmol) was dissolved in n-butanol (5 mL) and 6-chloro-9-(tetrahydropyran-2-yl)-9H-purine (0.54 g, 2.26 mmol) and DIPEA (2 mL, 11.3 mmol) added. The resultant dark red solution was heated to 100° C. overnight. The mixture was allowed to cool to RT and was concentrated in vacuo. The residue was purified by column chromatography (silica gel, gradient 0-10% MeOH in DCM) to afford 379 as a pale red solid (207 mg, 27%). LCMS (Method K): RT 2.68 min [M+H]+ 340.1 1H NMR (DMSO-d6, 400 MHz): δ 8.24 (1H, s), 8.15 (1H, s), 8.00-7.90 (1H, m), 7.64-7.55 (2H, m), 7.02 (1H, td, J=9.31, 2.40 Hz), 5.96-5.77 (1H, m), 4.98-4.85 (1H, m), 1.67 (3H, d, J=6.71 Hz), 1.57 (3H, d, J=6.91 Hz), 1.46 (3H, d, J=6.78 Hz)

1. temperatureto cool to RT
2. concentrationwas concentrated in vacuo
3. customThe residue was purified by column chromatography (silica gel, gradient 0-10% MeOH in DCM)