反応 #927236

ord-15557948ec354671bcc50160cab9f5a5

反応方程式

C#CCCCCCCOS(=O)(=O)c1ccc(C)cc1
7-octynyl-p-toluenesulfonate
[I-].[Na+]
sodium iodide
C#CCCCCCCI
8-iodo-1-octyne
収率 94.2%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他to react for four hours
  2. 2
    温度under reflux
  3. 3
    温度After cooling
  4. 4
    その他the precipitates were removed by filtration
  5. 5
    濃縮the filtrate was concentrated
  6. 6
    その他The resulting residue was purified by silica gel column chromatography (eluent; hexane)

実験手順

A mixture of 7-octynyl-p-toluenesulfonate (18.3 g, 65.2 mmol), sodium iodide (9.77 g, 65.2 mmol) and acetone (91 ml) was allowed to react for four hours under reflux. After cooling, the precipitates were removed by filtration, and the filtrate was concentrated. The resulting residue was purified by silica gel column chromatography (eluent; hexane) to afford 14.5 g of 8-iodo-1-octyne (yield; 94.2%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06365350B1uspto-grants-2002_04