反应详情

A solution of compound 19b (130 mg, 0.210 mmol) in MeOH (50 mL) was evacuated and back flushed with Argon gas three times before Pd/C (10%, 100 mg) was added. The mixture was evacuated and back flushed with H2, and was stirred at rt under H2 (in a balloon) for 3 h. The reaction mixture was filtered through a pad of diatomaceous earth, and the filtrate was concentrated under reduced pressure to leave a brown oil, which was purified by flash column chromatography on silica gel, eluting with EtOAc/heptane (0-100%). Compound 20a was obtained as an off-white solid (69.0 mg, 53% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C35H40N8O3: 621.3 (M+H). found: 621.4.

1. customback flushed with Argon gas three times before Pd/C (10%, 100 mg)
2. additionwas added
3. customThe mixture was evacuated
4. customback flushed with H2
5. filtrationThe reaction mixture was filtered through a pad of diatomaceous earth
6. concentrationthe filtrate was concentrated under reduced pressure
7. customto leave a brown oil, which
8. customwas purified by flash column chromatography on silica gel
9. washeluting with EtOAc/heptane (0-100%)