反应详情

温度

60 °C

To a solution of 2.1 g (7.0 mmol) of the quinazolinone prepared in Example 12 in 15 mL of dry DMF was added 1.74 g (20.0 mmol) of sodium acetate. The mixture was heated to 60° C. for 3 hours. The reaction mixture was concentrated in vacuo and the residue dissolved in 100 mL of CH2Cl2. The solution was washed with water (3×20 mL), brine (1×20 mL) and dried over MgSO4. The mixture was filtered and concentrated in vacuo. The residue was recrystallized from MeOH/H2O to give 1.31 g (4.8 mmol) of a colorless solid. 68% yield. 1H-NMR (CDCl3): 0.99 (t, 3H, J=7.32 Hz), 1.50 (m, 2H), 1.83 (m, 2H), 2.14 (t, 3H), 2.77 (3 line m, 2H, J=7.71 Hz), 5.23 (s, 2H), 7.69-7.78 (m, 2H), 8.25 (s, 1H), 10.90 (bs, 2H).

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionthe residue dissolved in 100 mL of CH2Cl2
3. washThe solution was washed with water (3×20 mL), brine (1×20 mL)
4. dry with materialdried over MgSO4
5. filtrationThe mixture was filtered
6. concentrationconcentrated in vacuo
7. customThe residue was recrystallized from MeOH/H2O