反应详情

In a flask flushed with nitrogen was added wet palladium on carbon (1.8 g) and a solution of Boc-D-Phe-D-Phe-D-Leu-OBn, intermediate 1-5 (11.1 g, 18.05 mmol) in methanol (50 μL). The mixture was stirred under a hydrogen balloon overnight. After filtration through celite, methanol was evaporated under reduced pressure. The residue was dissolved in acetone (20 mL) and slowly added to 500 mL water with 25 mL of 1N HCl under vigorous stirring. Pure product Boc-D-Phe-D-Phe-D-Leu-OH, intermediate 1-6 was obtained by filtration 9.4 g (99%). LC-MS: m/z=526 (M+H).

1. customIn a flask flushed with nitrogen
2. additionwas added wet palladium on carbon (1.8 g)
3. filtrationAfter filtration through celite, methanol
4. customwas evaporated under reduced pressure
5. dissolutionThe residue was dissolved in acetone (20 mL)
6. additionslowly added to 500 mL water with 25 mL of 1N HCl under vigorous stirring