反应详情

温度

160 °C

The product of Step 1 (100 mg) was dissolved in 1N KOH in MeOH (2 mL) and heated at 160° C. for 2 min via microwave irradiation. The resulting yellow solution was concentrated, diluted with water and acidified with 2N HCl. The precipitate was collected and recrystallised from EtOH/H2O to give 21 mg of product as colourless needles. 1H NMR (500 MHz, DMSO): 3.81 (3H, s), 7.08 (1H, t, J 7.4 Hz), 7.18 (1H, d J 7.4 Hz), 7.31 (1H, dd, J 1.2 and 8.0 Hz), 7.38 (1H, dd, J 1.2 and 8.0 Hz), 7.39-7.42 (1H, m), 7.44 (1H, s), 7.79 (1H, d, J 8.0 Hz). 7.89 (2H, d, J 8.5 Hz), 8.18 (2H, d, J 8.5 Hz), 10.76 (1H, s).

1. concentrationThe resulting yellow solution was concentrated
2. additiondiluted with water
3. customThe precipitate was collected
4. customrecrystallised from EtOH/H2O