反应详情

To a degassed solution of {4-[4-(3-tert-butoxycarbonylaminopropionylamino)phenyl]-butyl}carbamic acid benzyl ester 330 (1.78 g, 3.79 mmol) and methanol (50 mL) was added 10% palladium on activated carbon (0.5 g, 50% wet). The mixture was hydrogenated for 4 hours under atmospheric hydrogen. The catalyst was filtered through a pad of Celite and the solvent was evaporated in vacuo. The residue was purified by flash chromatography (silica gel, 6:1:0.1, v/v chloroform/methanol/concentrated ammonium hydroxide) to provide 340 (0.74 g, 58%). 1H NMR (300 MHz, CH3OD) δ 1.44 (s, 9H), 1.50 (m, 2H), 1.66 (m, 2H), 2.60 (m, 6H), 3.38 (m, 2H), 7.14 (d, 2H), 7.44 (d, 2H).

1. filtrationThe catalyst was filtered through a pad of Celite
2. customthe solvent was evaporated in vacuo
3. customThe residue was purified by flash chromatography (silica gel, 6:1:0.1, v/v chloroform/methanol/concentrated ammonium hydroxide)