反应详情

To a mixture of benzyl(3-(benzyloxy)-2-((3-(4-fluorophenyl)-2-oxopropyl)carbamoyl)-4-oxo-6,7,8,9-tetrahydro-7,10-ethanopyrimido[1,2-a]azepin-10(4H)-yl)carbamate, Intermediate 13 (540 mg, 0.845 mmol) in MeOH (8 mL) was added 1N HCl (0.930 mL, 0.930 mmol) followed by 10% Pd/C (90 mg, 0.085 mmol) and the mixture stirred under a hydrogen atmosphere for 2 h. The mixture was then filtered and thoroughly washed with ethyl acetate. The filtrate was concentrated in vacuo and dried under high vacuum overnight to afford the title compound (318 mg, 0.705 mmol, 83% yield) as an off-white solid. 1H NMR (500 MHz, DMSO-d6) δ ppm 12.07 (1H, br. s.), 9.61 (1H, t, J=5.95 Hz), 7.24-7.30 (2H, m), 7.13-7.20 (2H, m), 4.33 (2H, d, J=6.10 Hz), 4.00 (2H, d, J=3.66 Hz), 3.92 (2H, s), 2.46 (1H, br. s.), 2.01-2.13 (4H, m), 1.79-1.88 (2H, m), 1.68-1.77 (2H, m). LCMS (M+H)=415.15.

1. filtrationThe mixture was then filtered
2. washthoroughly washed with ethyl acetate
3. concentrationThe filtrate was concentrated in vacuo
4. customdried under high vacuum overnight