反应详情

温度

70 °C

The product of Example 130 (50 mg, 0.11 mmol) was stirred in DMF (0.3 mL). K2CO3 (45 mg, mmol, 0.33 mmol, 3 eq) and chloroacetamide (20 mg, 0.21 mmol, 2 eq) were added. The mixture was stirred at 70° C. for 2 h. EtOAc was added, washed with H2O and brine, dried over MgSO4, filtered, and concentrated. The residue was purified by Silica gel purification to yield the title compound. LC/MS (ESI+) 514.8 (M+H)+, tR=2.00 min (10–90% CH3CN/H2O in a 4-min run). 1H NMR (CDCl3) δ 87.46 (d, J=9.2 Hz, 2H), 7.27 (m, 4H), 6.91 (d, J=8.8 Hz, 2H), 4.12 (t, J=6.6 Hz, 2H), 3.81 (s, 3H), 3.15 (m, 4H), 2.29 (m, 3H), 0.97 (m, 2H), 0.87 (m, 2H) ppm.

1. washwashed with H2O and brine
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by Silica gel purification