反应详情

A solution containing 50 (0.53 mmol) and NH4OAc (25 mg, 0.27 mmol) in MeOH (10 mL) was treated with 10% Pd-on-carbon (wet, 60 mg, 0.05 mmol) and the stirred mixture was purged with hydrogen. After 1 h stirring under a balloon of hydrogen, TLC analysis (10:1 DCM/MeOH) indicated the reaction was complete. 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, 10-60% ACN/water containing 0.1% HOAc over 25 min; Flow: 40 mL/min). Fractions containing pure product were combined, frozen, and lyophilized to provide 251 mg (84%, 2 steps) of 51 as a floculent white powder.

1. customthe stirred mixture was purged with hydrogen
2. customThe catalyst was removed by filtration with an Acrodisc® 0.45 μm nylon membrane syringe
3. filtrationfilter
4. customthe solvent was removed in vacuo
5. customThe crude product was purified by reverse-phase HPLC (2″ Dynamax® C18, 10-60% ACN/water containing 0.1% HOAc over 25 min
6. additionFractions containing pure product
7. temperaturefrozen