反应详情

The product of Example 8B (200 mg, 0.50 mmol) in methanol (10 mL) was treated with Pd/C (Aldrich, 10% wt., 50 mg) at 60° C. under H2 for 10 hours. The mixture was allowed to cool to room temperature and was filtered through a short column of diatomaceous earth. The filtrate was concentrated under reduced pressure to provide the title compound (20 mg, yield, 13%). 1H NMR (MeOH-d4, 300 MHz) δ 1.43-1.56 (m, 1H), 1.62-1.88 (m, 2H), 1.99-2.12 (m, 1H), 2.14-2.21 (m, 1H), 2.79 (s, 3H) 2.90-3.03 (m, 5H), 3.27-3.38 (m, 1H), 4.49-4.56 (m, 1H), 6.67 (d, J=8.8, 2.7 Hz, 2H), 6.91 (d, J=8.8, 2.9 Hz, 2H), 7.35 (d, J=8.8, 2.7 Hz, 2H), 7.43 (d, J=9.2, 2.7 Hz, 2H) ppm. MS (DCl/NH3): m/z 309 (M+H)+.

1. filtrationwas filtered through a short column of diatomaceous earth
2. concentrationThe filtrate was concentrated under reduced pressure