反応 #7323

反応方程式

Pyridine

cyanuric fluoride

FMOC-Glycine

→

FMOC-glycyl fluoride

溶媒

dichloromethane

反応条件

後処理

1. 1
   ろ過the resulting slurry was filtered
2. 2
   workup.ADDITIONThe filtrate was poured into a separatory funnel
3. 3
   その他the layers were separated
4. 4
   乾燥The organic layer was dried over anhydrous sodium sulfate
5. 5
   ろ過filtered
6. 6
   濃縮concentrated under reduced pressure

実験手順

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%).

出典