反应详情

To a stirred solution of 5-(2-benzyloxy-phenyl)-isoxazole-3-carboxylic acid {2-[4-(2-chloro-phenoxy)-piperidin-1-yl]-2-oxo-ethyl}-amide (0.153 g, 0.00028 mole) in methanol (50 mL) was added 10% Pd/C (0.03 g) and the resulting mixture was stirred under an atmosphere of hydrogen for 3 hours. The mixture was then filtered through celite, the celite was washed with methanol and the organic layers were concentrated under reduced pressure. The resulting residue was purified by preparative HPLC to afford 0.055 g (43%) of 5-(2-hydroxy-phenyl)-isoxazole-3-carboxylic acid {2-[4-(2-chloro-phenoxy)-piperidin-1-yl]-2-oxo-ethyl}-amide. LCMS: 456.12 (M+1)+, 98.75%. 1H NMR (DMSO-d6): δ 10.8 (s, 1H), 8.7 (t, 1H), 7.8 (d, 1H), 7.4 (d, 1H), 7.24 (m, 3H), 7.12 (s, 1H), 7.04 (d, 1H), 6.92 (t, 2H), 4.7 (m, 1H), 4.2 (d, 2H), 3.7 (m, 2H), 3.4 (m, 2H), 1.9 (m, 2H), 1.6 (m, 2H).

1. filtrationThe mixture was then filtered through celite
2. washthe celite was washed with methanol
3. concentrationthe organic layers were concentrated under reduced pressure
4. customThe resulting residue was purified by preparative HPLC