反应详情

To a mixture of benzyl (2-((4-fluorobenzyl)carbamoyl)-3-hydroxy-4-oxo-6,7,8,9-tetrahydro-7,10-ethanopyrimido[1,2-a]azepin-10(4H)-yl)carbamate (300 mg, 0.59 mmol) in methanol (3 mL) was added 10% Pd/C (315 mg) and the mixture was stirred under balloon hydrogen atmosphere for 18 h. The mixture was then filtered through a pad of CELITE® and the pad washed with ethyl acetate. The filtrate was concentrated to afford the title compound (160 mg, 72% yield) as a light yellow solid. 1H NMR (500 MHz, DMSO-d6) δ: 12.22 (s, 1H), 9.50 (brs, 1H), 7.35-7.41 (m, 2H), 7.19-7.22 (m, 2H), 4.54 (d, 2H, J=5.8 Hz), 4.01 (s, 2H), 2.42-2.48 (m, 3H), 2.08 (s, 2H), 1.98-2.03 (m, 2H), 1.84-1.90 (m, 2H), 1.70-1.78 (m, 2H). LCMS (M+H)=373.28.

1. filtrationThe mixture was then filtered through a pad of CELITE®
2. washthe pad washed with ethyl acetate
3. concentrationThe filtrate was concentrated