反应详情

To a mixture of ethyl 10-amino-4-oxo-3-((phenylcarbonyl)oxy)-4,6,7,8,9,10-hexahydro-7,10-ethanopyrimido[1,2-a]azepine-2-carboxylate hydrochloride (6 g, 11.96 mmol) in ethyl acetate (100 mL) and ethanol (100 mL) was added 1N HCl (12.56 mL, 12.56 mmol) followed by Pd/C (1.273 g, 1.196 mmol) and the mixture stirred under 1 atm of hydrogen for 2 h. The mixture was then filtered (filter paper) and the solid thoroughly washed with ethyl acetate. The filtrate was concentrated under reduced pressure and dried under high vacuum overnight to afford the title compound (4.8 g, 90% yield)as an off-white solid. 1H NMR (500 MHz, CDCl3) δ: 8.15 (2 H, d, J=7.28 Hz), 7.62-7.67 (1 H, m), 7.47-7.52 (2 H, m), 4.26 (2 H, q, J=7.03 Hz), 4.11 (2 H, d, J=3.76 Hz), 2.76 (3 H, s), 2.56 (1 H, brs), 2.16-2.25 (2 H, m), 2.00-2.13 (4 H, m), 1.68-1.82 (3 H, m), 1.12 (3 H, t, J=7.03 Hz). LCMS (M+H)=412.78.

1. filtrationThe mixture was then filtered
2. filtration(filter paper)
3. washthe solid thoroughly washed with ethyl acetate
4. concentrationThe filtrate was concentrated under reduced pressure
5. customdried under high vacuum overnight