反应 #7326

ord-9c73895b2c0a498e9c55ac238f8665f2

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the resulting slurry was filtered
  2. 2
    workup.ADDITIONThe filtrate was poured into a separatory funnel
  3. 3
    其他the layers were separated
  4. 4
    干燥The organic layer was dried over anhydrous sodium sulfate
  5. 5
    过滤filtered
  6. 6
    浓缩concentrated under reduced pressure

实验过程

FMOC-L-Leucine (5 g, 14.14 mmol) (Bachem) was dissolved in acetonitrile (70 mL). Pyridine (1.14 mL, 14.14 mmol) (Aldrich) and cyanuric fluoride (1.91 g, 14.14 mmol) (Aldrich) were successively added at room temperature and the mixture was stirred overnight. Ice cold water (300 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-L-leucyl fluoride as a white powder. (Yield 4.57 g, 91%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07084270B2uspto-grants-2006_08