Reaktion #40358

ord-f8ba92078b904485847e2987af2a83d5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeIn a flask flushed with nitrogen
  2. 2
    workup.ADDITIONwas added wet palladium on carbon (1.8 g)
  3. 3
    FiltrationAfter filtration through celite, methanol
  4. 4
    Sonstigewas evaporated under reduced pressure
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in acetone (20 mL)
  6. 6
    workup.ADDITIONslowly added to 500 mL water with 25 mL of 1N HCl under vigorous stirring

Vorschrift

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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07727963B2uspto-grants-2010_06