反応 #651853

ord-574ac1b8ab2e4ef1a751a2914dbc0520

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    温度under reflux
  3. 3
    温度by heating for 7 hours
  4. 4
    抽出extracted with toluene
  5. 5
    その他The organic layer thus obtained
  6. 6
    洗浄was washed with water
  7. 7
    その他dried
  8. 8
    濃縮concentrated under a reduced pressure
  9. 9
    その他to obtain a brown oily product
  10. 10
    その他This product was isolated
  11. 11
    その他purified

実験手順

To 30 ml of N-methylpyrrolidone was dissolved 3 g of 2-(trans-4-propylcyclohexyl)ethenyl bromide, 2 g of copper cyanide was added thereto, and then stirred under reflux by heating for 7 hours. A solution of ferric chloride in 6N hydrochloric acid was added to the reaction liquid, and extracted with toluene. The organic layer thus obtained was washed with water, dried, and then concentrated under a reduced pressure to obtain a brown oily product. This product was isolated and purified by using silica gel column chromatography to obtain 1.5 g of an oily product. As a result of various instrumental analysises, the product was confirmed to be the subject compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06168839Auspto-grants-2001_01