반응 #7323

ord-8e925202aa5c48a68b53aa693faeea25

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과the resulting slurry was filtered
  2. 2
    workup.ADDITIONThe filtrate was poured into a separatory funnel
  3. 3
    기타the layers were separated
  4. 4
    건조The organic layer was dried over anhydrous sodium sulfate
  5. 5
    여과filtered
  6. 6
    농축concentrated under reduced pressure

실험 절차

FMOC-Glycine (5.02 g, 16.82 mmol) (Bachem) was dissolved in dichloromethane (85 mL). Pyridine (1.36 mL, 16.82 mmol) (Aldrich) and cyanuric fluoride (2.27 g, 16.82 mmol) (Aldrich) were successively added at room temperature and the mixture was stirred overnight. 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-glycyl fluoride as a white powder. (Yield 3.67 g, 73%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084270B2uspto-grants-2006_08