反应详情

A solution containing 46 (4.10 g, 7.02 mmol) and NH4OAc (275 mg, 3.50 mmol) in MeOH (70 mL) was treated with 10% Pd-on-carbon (wet, 745 mg, 0.70 mmol) and the stirred mixture was purged with hydrogen. After 3 h stirring under a balloon of hydrogen, TLC analysis (1:1 hexanes/EtOAc) indicated the reaction was complete. The catalyst was removed by filtration and the solvent was concentrated in vacuo. The residue was dissolved in Et2O and washed successively with saturated aqueous NaHCO3 and brine, dried over anhydrous Na2SO4, filtered, and concentrated to provide 3.30 g of 47 as colorless oil which was used without further purification. Mass spectrum, m/z [449.9] (M+H)+.

1. customthe stirred mixture was purged with hydrogen
2. customThe catalyst was removed by filtration
3. concentrationthe solvent was concentrated in vacuo
4. dissolutionThe residue was dissolved in Et2O
5. washwashed successively with saturated aqueous NaHCO3 and brine
6. dry with materialdried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated