反应详情

温度

65 °C

A solution of Intermediate 14h (57 mg, 0.08 mmol) and dimethylamine (2M in THF, 0.873 mL, 1.75 mmol) in THF (4 mL) was heated at 60° C. for 18 h. A further 1.4 mL of dimethylamine (2M in THF) was added and the reaction mixture was heated at 65° C. for 48 h. The reaction mixture was cooled to RT and the solvent was removed by air, to leave a residue which was purified by MDAP (Method 7), to afford the title compound (18 mg, 35%). LCMS (Method 5): Rt: 3.00 min, m/z 600.4 [MH+]. 1H NMR (400 MHz, d6-DMSO): 1.20 (9H, s), 1.32-1.47 (2H, m), 1.64-1.76 (1H, m), 1.76-1.86 (211, m), 1.87-2.12 (4H, m), 2.13-2.21 (9H, m), 2.86-2.99 (2H, m, obscured by water), 3.35-3.48 (2H, m, obscured by water), 3.57 (2H, s, obscured by water), 4.82-4.91 (1H, m), 5.57 (1H, t, J=4.5 Hz), 6.02 (1H, s), 6.91 (1H, d, J=8.8 Hz), 7.18 (1H, dd, J=9.8, 1.9 Hz), 7.26-7.33 (1H, m), 7.34-7.43 (3H, m), 7.62 (1H, d, J=10.0 Hz), 7.65 (1H, d, J=1.8 Hz), 8.19 (1H, s), 8.27 (1H, s).

1. temperatureThe reaction mixture was cooled to RT
2. customthe solvent was removed by air
3. customto leave a residue which
4. customwas purified by MDAP (Method 7)