反应 #65922

ord-bcd683ca1d504603831d112f5f722637

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05420348uspto-grants-1995_05