反应详情

To 122C (1 g, 4 mmol) in acetone (20 mL) was added K2CO3 (1.64 g) and iodomethane (0.75 mL). The mixture was stirred at rt for 3 h. After TLC (10% EtOAc/Hexane) indicated the reaction was complete, the mixture was diluted with diethyl ether, washed with water and brine. The organic layer was dried over MgSO4 and concentrated. The crude product was purified by silica gel chromatography to give 122D (0.75 g, 70% yield). 1H NMR (400 MHz, CDCl3) δ ppm 2.16 (s, 3H) 3.78 (s, 3H) 6.85 (d, J=8.79 Hz, 1H) 7.05 (d, J=5.27 Hz, 1H).

1. washwashed with water and brine
2. dry with materialThe organic layer was dried over MgSO4
3. concentrationconcentrated
4. customThe crude product was purified by silica gel chromatography