反应详情

Intermediate 56 (2.1 g, 5.4 mmol) was dissolved in Dioxane (30 ml) and added POCl3 (1.5 ml). This mixture was refluxed for 5 h. After 5 h, dioxane was removed on rotavapour to obtain the residue. Work up (EtOAc/H2O) of the residue afforded the crude. Crude was purified by column on 60-120 mesh silica gel using DCM as eluent to afford the titled compound (1.2 g). 1H-NMR (δ ppm, CDCl3, 400 MHz): 8.46 (d, J 2.1, 1H), 8.41 (d, J 8.2, 2H), 8.24 (d, J 2.1, 1H), 7.83 (d, J 8.2, 2H).

1. temperatureThis mixture was refluxed for 5 h
2. customdioxane was removed on rotavapour
3. customto obtain the residue
4. customafforded the crude
5. customCrude was purified by column on 60-120 mesh silica gel