反応 #2501396

ord-65259a8d9eb74c7cbd2cbf84a81bfdb2

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling down
  2. 2
    その他the mixture vigorously stirred overnight
  3. 3
    ろ過Filtration
  4. 4
    洗浄washing with ether
  5. 5
    その他yielded a brown solid, which
  6. 6
    ろ過the solution filtered
  7. 7
    その他the water removed in vacuo
  8. 8
    ろ過the mixture filtered
  9. 9
    洗浄the residue washed with ethyl ether

実験手順

Di(1-naphthyl)sulfide (3 g, 0.0104 mole), diphenyliodonium triflate (5.8 g, 0.0135 mole) and copperbenzoate (0.08 g, 0.003 mole) are heated without solvent for 3 hours at 120-145° C. under a nitrogen atmosphere. After cooling down, 75 ml ether was added and the mixture vigorously stirred overnight to achive solidification. Filtration and washing with ether yielded a brown solid, which was dissolved in hot water, the solution filtered and the water removed in vacuo. The resulting white solid was stirred in 50 ml ethyl ether for 24 hours, the mixture filtered and the residue washed with ethyl ether, yielding 4.8 g (90%) of the title compound, di-(1-naphtyl)phenylsulfonium triflate. The structure was confirmed by 1H/13C NMR spectroscopy.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06811961B2uspto-grants-2004_11