反应详情

The product of Step 6 (0.2 g), in a mixture of concentrated HCl (2 mL) and EtOH (3 mL), was heated at reflux for 1 h. The mixture was concentrated and the residue crystallized from EtOH/H2O to give 70 mg of product as a colourless solid. 1H NMR (360 MHz, CDCl3): 7.33 (1H, s), 7.39 (1H, d, J 8.0 Hz), 7.43 (1H, s), 7.5-7.55 (1H, m), 7.73 (2H, d, J 8.0 Hz), 7.99 (1H, d, J 8.0 Hz), 8.09 (2H, d, J 8.0 Hz), 8.14 (1H, d, J 8.0 Hz), 8.9 (1H, d, J 8.0 Hz).

1. temperaturewas heated
2. temperatureat reflux for 1 h
3. concentrationThe mixture was concentrated
4. customthe residue crystallized from EtOH/H2O