反应详情

温度

90 °C

A mixture of 6-bromo-9H-purine (74 mg, 0.37 mmol), 1-[5-chloro-8-(3-fluorophenyl)isoquinolin-7-yl]ethanamine (0.075 g, 0.25 mmol), and N,N-diisopropylethylamine (0.087 mL, 0.50 mmol) in isopropyl alcohol (2 mL) was heated at 90° C., under nitrogen, overnight. The mixture was evaporated and the resulting mixture was purified on a RP-HPLC (XBridge C18 column, eluting with a gradient of acetonitrile in water with 0.2% ammonium hydroxide, at a flow rate of 30 mL/min) to give the desired product. LCMS calculated for C22H17ClFN6 (M+H)+: m/z=419.1; Found: 419.1. 1H NMR (DMSO-d6, 400 MHz) δ 8.58 (2H, m), 8.30 (2H, m), 8.06 (1H, s), 8.00 (1H, d, J=5.2 Hz), 7.92 (1H, d, J=6.0 Hz), 7.58 (2H, m), 7.37˜7.20 (2H, m), 5.19 (1H, m), 3.29 (1H, br s), 1.39 (3H, m) ppm. 19F NMR (DMSO-d6, 376 MHz) δ −113.5 ppm.

1. customThe mixture was evaporated
2. customthe resulting mixture was purified on a RP-HPLC (XBridge C18 column
3. washeluting with a gradient of acetonitrile in water with 0.2% ammonium hydroxide, at a flow rate of 30 mL/min)