反应详情

温度

80 °C

To a solution of Compound (2) (13 mg, 26 μmol) in ACN (1 mL) was added potassium carbonate (7.3 mg, 52 μmol) followed by 2-bromoethanol (5.6 μL, 79 μmol). The mixture was then stirred at 80° C. for 16 h (monitored by LCMS). The mixture was cooled to RT, diluted with EtOAc (3 mL), washed with water (1 mL) and brine (2 mL). The organic phase was dried (MgSO4) and the solvent was removed in vacuo. The crude mixture was purified by preparative HPLC to give Compound (3) (4.86 mg, 34%) as a white powder. ESI-MS m/z calculated for [M+H]+: 539.18; found: 539.12; 1H NMR (400 MHz, CDCl3) δ 7.80 (s, 1H), 7.52 (brd, J=9.0 Hz, 2H), 7.47 (s, 1H), 7.12-7.02 (m, 6H), 5.79 (brd, J=4.3 Hz, 1H), 4.21-4.00 (m, 1H), 3.85-3.62 (m, 3H), 3.18 (s, 3H), 2.99 (d, J=4.9 Hz, 3H), 2.51-2.27 (m, 1H), 1.06 (ddd, J=11.3, 6.9, 3.1 Hz, 3H), 0.62-0.44 (m, 1H).

1. temperatureThe mixture was cooled to RT
2. washwashed with water (1 mL) and brine (2 mL)
3. dry with materialThe organic phase was dried (MgSO4)
4. customthe solvent was removed in vacuo
5. customThe crude mixture was purified by preparative HPLC