反应详情

温度

23 °C

To a solution of 4.3 (0.0241 g, 0.0521 mmol) in THF/MeOH (2/1) (1.5 mL) was added LiOH (0.50 mL, 0.500 mmol). The resulting mixture was stirred overnight at 23° C., quenched with excess 1N HCl, and extracted with EtOAc. The combined organic layers were dried over Na2SO4 and concentrated. The crude residue was purified by combiflash (0 to 40% EtOAc/hexanes) to afford 4 (0.0166 g, 71.0% yield). MS ESI (neg.) m/e: 393.1 (M−H)+. 1H NMR (400 MHz, CDCl3) δ ppm 7.32 (1H, s), 7.20-7.29 (4H, m), 6.83-6.92 (5H, m), 6.74 (1H, d, J=2.9 Hz), 5.07 (2H, s), 3.83 (2H, t, J=6.6 Hz), 3.79 (3H, s), 2.97 (2H, t, J=7.8 Hz), 2.68-2.73 (2H, m), 2.19 (3H, s), 1.53-1.60 (2H, m), 1.22-1.31 (2H, m), 0.83 (3H, t, J=7.3 Hz).

1. customquenched with excess 1N HCl
2. extractionextracted with EtOAc
3. dry with materialThe combined organic layers were dried over Na2SO4
4. concentrationconcentrated
5. customThe crude residue was purified by combiflash (0 to 40% EtOAc/hexanes)