反应详情

A mixture of 2-{[2-(benzyloxy)-4,6-dimethylpyridin-3-yl]methyl}-N,N,8-trimethyl-1-oxo-1,2,3,4-tetrahydroisoquinoline-7-carboxamide (76f, 80 mg, 0.175 mmol) and 10% Pd/C (10 mg) in MeOH (10 mL) was hydrogenated under H2 balloon at room temperature for 20 hours. The mixture was filtered and the solids were washed with MeOH (2×10 mL). The filtrate was concentrated under vacuum and the residue was purified by column chromatography (EtOAc/MeOH=5:1) to give the title compound (Example 76, 32 mg, 49.7%) as a white solid. 1H NMR (400 MHz, methanol-d4) δ 7.22-7.2 (d, 1H), 7.17-7.15 (d, 1H), 6.11 (s, 1H), 4.77 (s, 2H), 3.45-3.43 (m, 2H), 3.13 (s, 3H), 2.9-2.85 (m, 5H), 2.28 (s, 3H), 2.25 (s, 3H); MS 367.9 [M+H].

1. customat room temperature
2. customfor 20 hours
3. filtrationThe mixture was filtered
4. washthe solids were washed with MeOH (2×10 mL)
5. concentrationThe filtrate was concentrated under vacuum
6. customthe residue was purified by column chromatography (EtOAc/MeOH=5:1)