反应详情

The product of step 2 (4.5 g, 13 mmol) and K2CO3 (18 g, 130 mmol) was heated at reflux for 5 h in 50% aqueous ethanol. The mixture was cooled and concentrated, and the residue partitioned between water (50 ml) and dichloromethane (100 ml). The organic extract was dried (MgSO4) and solvent removed. The residual solid was recrystallized from hexane/ethyl acetate to afford 3.2 g (91%) of the title compound. m.p.: 128-130° C. 1H-NMR (CDC13) δ: 7.85-7.76 (2H, m), 7.64 (1H, br s), 7.59-7.49 (4H, m), 7.22 (1H, d, J=1.8 Hz), 7.02 (1H, dd, J=1.8, 8.4 Hz), 5.60 (2H, br s).

1. temperatureThe mixture was cooled
2. concentrationconcentrated
3. customthe residue partitioned between water (50 ml) and dichloromethane (100 ml)
4. extractionThe organic extract
5. dry with materialwas dried (MgSO4) and solvent
6. customremoved
7. customThe residual solid was recrystallized from hexane/ethyl acetate