反应详情

Compound 29d (100 mg, 0.147 mmol) in MeOH (15 mL) and DCM (5 mL) was hydrogenated over 10% Pd/C (20 mg) overnight under balloon pressure. The reaction mixture was filtered through a pad of diatomaceous earth and the filtrate was concentrated and dried under reduced pressure to obtain the title compound 99. 1H-NMR (400 MHz, DMSO-d6) δ (ppm): 8.36 (d, J=2.3 Hz, 1H), 8.04 (d, J=9.0 Hz, 1H), 7.84-7.92 (m, 2H), 7.71 (d, J=7.8 Hz, 1H), 7.49-7.60 (m, 2H), 7.33-7.37 (m, 1H), 7.19-7.25 (m, 1H), 7.03 (d, J=8.6 Hz, 1H), 6.77 (d, J=9.0 Hz, 1H), 5.77 (s, 1H), 4.44-4.52 (m, 2H), 4.24 (t, J=6.8 Hz, 2H), 4.10-4.20 (m, 4H), 3.68-3.78 (m, 8H), 3.36 (br. s., 2H), 2.97-3.10 (m, 2H), 2.56 (br. s., 1H). Mass Spectrum (LCMS, ESI pos.) Calcd. for C31H33N9O: 548.3 (M+H). Found 548.3.

1. filtrationThe reaction mixture was filtered through a pad of diatomaceous earth
2. concentrationthe filtrate was concentrated
3. customdried under reduced pressure