反应详情

温度

130 °C

Into a 25-mL round-bottom flask was placed a solution of (S)-1-(1-phenyl-1H-benzo[d]imidazol-2-yl)ethanamine from Example 4 (238 mg, 1.00 mmol, 1.00 equiv) in n-BuOH (8 mL), 4-chloro-5H-pyrrolo[3,2-d]pyrimidine from Example 20 (155 mg, 0.99 mmol, 0.99 equiv, 98%) and N-ethyl-N-isopropylpropan-2-amine (400 mg, 3.03 mmol, 3.02 equiv, 98%). The resulting solution was stirred overnight at 130° C. and concentrated under vacuum. The residue was purified by applying onto a C18 column eluted with water/acetonitrile (95:5-20:80) to afford 150 mg (41%) of 147 as a light-yellow solid. LC-MS (ES, m/z): 355 [M+H]+. 1H-NMR (300 MHz, CD3OD, ppm): δ 8.49 (s, 1H), 7.85-7.48 (m, 9H), 7.32-7.30 (m, 1H), 6.63 (d, 1H), 5.81-5.74 (m, 1H), 1.89 (d, 3H)

1. customInto a 25-mL round-bottom flask was placed
2. concentrationconcentrated under vacuum
3. customThe residue was purified
4. washeluted with water/acetonitrile (95:5-20:80)