반응 #651853

ord-574ac1b8ab2e4ef1a751a2914dbc0520

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    온도under reflux
  3. 3
    온도by heating for 7 hours
  4. 4
    추출extracted with toluene
  5. 5
    기타The organic layer thus obtained
  6. 6
    세척was washed with water
  7. 7
    기타dried
  8. 8
    농축concentrated under a reduced pressure
  9. 9
    기타to obtain a brown oily product
  10. 10
    기타This product was isolated
  11. 11
    기타purified

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06168839Auspto-grants-2001_01