反应详情

温度

45 °C

To a stirred mixture of 66.46C (0.73 g, 2.30 mmol) in MeOH (10 mL) was added PPTS (58.8 mg, 0.234 mmol). The mixture was heated to 45° C. and monitored with TLC and LCMS. After 19 hours, the organic solvent was removed under reduced pressure and the residue was purified on silica gel (0-25% EtOAc in hexanes) to afford 66.46D (361 mg, 67% yield). 1H NMR (400 MHz, CDCl3) δ ppm 7.87 (2H, td, J=8.7, 2.2 Hz), 6.95 (1H, d, J=8.6 Hz), 6.00 (1H, m), 5.94 (1H, s), 4.34 (2H, q, J=2.7 Hz), 3.97 (2H, t, J=5.5 Hz), 3.89 (3H, s), 2.47 (2H, ddd, J=9.8, 5.5, 2.7 Hz).

1. customthe organic solvent was removed under reduced pressure
2. customthe residue was purified on silica gel (0-25% EtOAc in hexanes)