反応 #65922

反応方程式

2-Acetylfluorene

cycloheptylamine

ethanol

sodium borohydride

→

amine

収率 25.9%

N-Cycloheptyl-1-(2-fluorenyl)ethylamine

収率 25.9%

溶媒

water

反応条件

後処理

1. 1
   workup.DISTILLATIONdistilled under reduced pressure
2. 2
   抽出extracted with chloroform (80 ml×2 times)
3. 3
   乾燥The organic layer was dried over anhydrous magnesium sulfate
4. 4
   濃縮concentrated
5. 5
   その他The residue was then purified by silica gel column chromatography

実験手順

2-Acetylfluorene (4.17 g, 20 mmol) and cycloheptylamine (2.38 g, 21 mmol) were heated together at 130° C. for 14 hrs and, then, distilled under reduced pressure. To the residue were added ethanol (20 ml) and sodium borohydride (0.76 g, 20 mmol) and the mixture was stirred at room temperature overnight. The mixture was then diluted with water (100 ml) and extracted with chloroform (80 ml×2 times). The organic layer was dried over anhydrous magnesium sulfate and concentrated. The residue was then purified by silica gel column chromatography to give 1.58 g of the amine compound.

出典