反应详情

温度

140 °C

A 25 mL sealed tube was charged with 101b (300 mg, 0.88 mmol), 101l (423 mg, 0.88 mmol), Cs2CO3 (572 mg, 1.76 mmol), Pd2(dba)3 (80 mg, 0.09 mmol) suspended in CH3CN (25 mL), and H2O (1 mL). The mixture was heated at 140° C. under microwave irradiation for 1 hour. It was then evaporated and the residue was purified by silica-gel column eluting with 10:1 methylene chloride/methanol to give the crude product, which was further purified by reverse phase Combi-flash eluting with 0.3% NH4HCO3 in 1:4 water/CH3CN to afford 101 as a yellow solid (150 mg, 28%). MS: (M+H)+ 621. 1H NMR (500 MHz, DMSO) δ 8.94 (s, 1H), 8.27 (d, J=1.5, 1H), 8.16 (d, J=1.5, 1H), 7.96 (d, J=1.0, 1H), 7.91 (d, J=2.5, 1H), 7.58 (d, J=1.5, 1H), 7.33-7.42 (m, 3H), 7.25-7.28 (m, 1H), 6.53 (s, 1H), 4.88 (t, J=4.5, 1H), 4.30 (d, J=4.5, 2H), 4.12-4.20 (m, 3H), 3.90-3.92 (m, 1H), 3.06 (t, J=4.5, 4H), 2.53-2.65 (m, 2H), 2.43-2.48 (m, 6H), 2.21 (s, 3H), 1.76-1.81 (m, 2H), 1.67-1.71 (m, 2H)

1. customA 25 mL sealed tube
2. customIt was then evaporated
3. customthe residue was purified by silica-gel column
4. washeluting with 10:1 methylene chloride/methanol
5. customto give the crude product, which
6. customwas further purified by reverse phase Combi-flash
7. washeluting with 0.3% NH4HCO3 in 1:4 water/CH3CN