反应详情

A solution of the product of Step 3 (2.4 g, 0.0064 mol) in 1M KOH in MeOH (16 mL) was heated at 150° C. in a sealed tube via microwave irradiation for 15 min. The mixture was then concentrated, diluted with H2O, acidified with 1N HCl and the resulting precipitate collected by filtration to give 1.0 g (44% yield) of product. 1H NMR (360 MHz, CDCl3): 7.37 (1H, dd, J 1.4 and 8.5 Hz), 7.66 (1H, d, 1.4 Hz), 7.73 (1H, d, 8.5 Hz), 7.89 (2H, d, 8.5 Hz), 8.13 (2H, d, 8.5 Hz), 11.0 (1H, s).

1. concentrationThe mixture was then concentrated
2. additiondiluted with H2O
3. filtrationthe resulting precipitate collected by filtration