反应详情

A solution of the product of Step 2 (3 g, 0.0078 mol) in SOCl2 (15 mL) was heated at reflux for 24 h. The mixture was then concentrated and the residue partitioned between ether (3×20 mL) and Na2CO3 solution (10 mL). The organic phase was separated, dried (MgSO4) and concentrated to give 2.5 g (85% yield) of product as a tan powder. 1H NMR (360 MHz, CDCl3): 7.25 (1H, d, J 8.9 Hz), 7.37 (1H, d, 8.9 Hz), 7.80-7.95 (5H, m).

1. temperatureat reflux for 24 h
2. concentrationThe mixture was then concentrated
3. customthe residue partitioned between ether (3×20 mL) and Na2CO3 solution (10 mL)
4. customThe organic phase was separated
5. dry with materialdried (MgSO4)
6. concentrationconcentrated