反应详情

A solution of 3.2 (1.86 g, 5.5 mmol) and 10% Pd/C (440 mg) in dry THF (30 ml) was stirred under H2 for 16 hrs. The resulting mixture was filtered through celite which was washed with EtOAc (40 ml) and the filtrate was concentrated. The residue was purified by chromatography (SiO2, 0 to 40% EtOAc in hexanes) to afford 3.3 (1.63 g, 96%) as a bright yellow oil. 1H NMR (250 MHz, CDCl3) δ ppm 7.40-7.72 (m, 6H), 7.18 (s, 1H), 6.92 (d, 1H), 6.82 (dd, 1H), 3.92 (q, 2H), 3.68 (br s, 2H), 1.06 (t, 3H); FABMS: (NBA/NaI) m/z 308 (M+H+ expected 308).

1. filtrationThe resulting mixture was filtered through celite which
2. washwas washed with EtOAc (40 ml)
3. concentrationthe filtrate was concentrated
4. customThe residue was purified by chromatography (SiO2, 0 to 40% EtOAc in hexanes)