反应详情

Composition 13 (163 mg, 0.33 mmol) and MeOH (˜15 mL) was added to a dry round bottom flask equipped with a magnetic stir bar. The flask was purged several times with N2 and a catalytic amount of 10% Pd on C was carefully added to the reaction flask. The resulting black heterogeneous mixture was evacuated under vacuum and charged twice with H2 via a rubber balloon with constant stirring. The reaction was stirred at room temperature for 1.5 h and upon completion was filtered thru a pad of Celite, concentrated in vacuo to give 14 (115 mg, 0.32 mmol, 99% yield) as a sticky off-white solid. ESMS: 354.8 (M+H), 376.2 (M+Na+).

1. customequipped with a magnetic stir bar
2. customThe flask was purged several times with N2
3. additiona catalytic amount of 10% Pd on C was carefully added to the reaction flask
4. customThe resulting black heterogeneous mixture was evacuated under vacuum
5. additioncharged twice with H2 via a rubber balloon with constant stirring
6. filtrationwas filtered
7. concentrationconcentrated in vacuo