反应详情

3B (290 mg, 0.9 mmol) was hydrogenated in EtOH (9.0 mL) and HOAc (0.15 mL) with Pt/C (5% wt, 100 mg) using a H2 balloon for 2 days. After filtration and evaporation of solvent, the crude product was stirred in EtOAc (1.0 mL) and 4.0 N HCl/dioxane (4.3 mL, 18 eq) at rt for 1.0 h. After removal of solvent, 3C was obtained as HCl salt. 1H NMR (400 MHz, Methanol-d4) δ ppm 2.26 (m, 3H) 2.55 (m, 1H) 3.49 (m, 2H) 4.74 (dd, J=10.11, 6.59 Hz, 1H) 7.66 (t, J=7.69 Hz, 1H) 7.74 (m, 1H) 7.97 (d, J=7.91 Hz, 1H) 8.04 (s, 1H).

1. customfor 2 days
2. filtrationAfter filtration and evaporation of solvent
3. customAfter removal of solvent