反应详情

A mixture of 58 (250 mg, 0.37 mmol) and 10% Pd-on-carbon (wet, 100 mg, 0.10 mmol) in MeOH (10 mL) was stirred vigorously under an atmosphere of H2. After 3.5 h, the catalyst was removed by filtration with an Acrodisc® 0.45 μm nylon membrane syringe filter and the solvent was removed in vacuo. The crude product was purified by reverse-phase HPLC (2″ Dynamax® C18, 20-80% MeOH/water containing 0.1% HOAc over 25 min; Flow: 40 mL/min). The product-containing fractions were combined and lyophilized to provide 59 (130 mg, 65%) as a flocculent white powder.

1. customthe catalyst was removed by filtration with an Acrodisc® 0.45 μm nylon membrane syringe
2. filtrationfilter
3. customthe solvent was removed in vacuo
4. customThe crude product was purified by reverse-phase HPLC (2″ Dynamax® C18, 20-80% MeOH/water containing 0.1% HOAc over 25 min