Reaktion #7331

ord-ff701405dbdb4c8d96cc24948af218ae

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe resulting slurry was filtered
  2. 2
    workup.ADDITIONThe filtrate was poured into a separatory funnel
  3. 3
    Sonstigethe layers were separated
  4. 4
    TrocknenThe organic layer was dried over anhydrous sodium sulfate
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated under reduced pressure

Vorschrift

FMOC-D-Methionine (5.00 g, 13.46 mmol) (Bachem) was dissolved in dichloromethane (70 mL). Pyridine (1.09 mL, 13.46 mmol) (Aldrich) and cyanuric fluoride (1.82 g, 13.46 mmol) (Aldrich) were successively added at room temperature and the mixture was stirred for 4 hours. Ice cold water (100 mL) was added and the resulting slurry was filtered. The filtrate was poured into a separatory funnel and the layers were separated. The organic layer was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to afford FMOC-D-methionyl fluoride as a white powder. (Yield 3.7 g., 74%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07084270B2uspto-grants-2006_08