反应 #1701299

ord-66db2f99b61547f9a400e2559cab4e07

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度is heated
  2. 2
    温度under reflux for 24 hours (compare T. Ishihara, Chemistry Letters (1986) 1895)
  3. 3
    workup.ADDITIONThe isomer mixture of the addition product
  4. 4
    其他thus formed
  5. 5
    过滤after the catalyst has been filtered off
  6. 6
    温度first heated with tributyl-tin hydride for 90 hours in toluene

实验过程

A mixture of 0.1 mol of 4-(trans-4-propylcyclohexyl)-cyclohex-1-ene, 0.1 mol of heptafluoropropyl iodide, 10 mol % of tetrakis-(triphenylphosphine)-palladium and 200 ml of hexane is heated under reflux for 24 hours (compare T. Ishihara, Chemistry Letters (1986) 1895). The isomer mixture of the addition product thus formed is, after the catalyst has been filtered off, first heated with tributyl-tin hydride for 90 hours in toluene and reduced. The all-trans product, trans-4-(trans-4-propylcyclohexyl)-1-heptafluoropropylcyclohexane, is finally obtained by separating the thiourea inclusion compound from a solution in methanol.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05196140uspto-grants-1993_03