反应详情

The product of Example 28D (200 mg, 0.59 mmol) was hydrogenated under the catalysis of Pd/C (Aldrich, 10 wt. %, 50 mg) in EtOH (10 mL) under hydrogen at ambient temperature for 10 h. After the reaction went to completion, the catalyst was removed through a short column of diatomaceous earth (˜2 g) and the filtrate was washed with EtOH (2×5 mL). The ethanol solution was concentrated to give the title compound (180 mg, yield, 98%). 1H NMR (500 MHz, CD3-OD) δ 1.58-1.73 (m, 1H), 1.76-2.00 (m, 2H), 2.06-2.27 (m, 1H), 2.29-2.47 (m, 1H), 2.81-3.20 (m, 5H), 3.52-3.68 (m, 1H), 5.11-5.57 (m, 1H), 6.78 (d, J=8.2 Hz, 1H), 7.12-7.26 (m, 2H), 7.32 (d, J=2.1 Hz, 1H), 7.92 (d, J=9.2 Hz, 1H) ppm. MS (DCI/NH3): 312 (M+H)+.

1. customthe catalyst was removed through a short column of diatomaceous earth (˜2 g)
2. washthe filtrate was washed with EtOH (2×5 mL)
3. concentrationThe ethanol solution was concentrated