Reaktion #497187

ord-000adc2683c1418aa85492f8cfdf5de8

Reagenzien

Keine

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigereacted at −78° C. for 40 minutes under
  2. 2
    Sonstigea dry
  3. 3
    Sonstigeanaerobic operation condition to form a solution
  4. 4
    Sonstigereacted at −78° C. for 1 hour
  5. 5
    SonstigeAfter returning to room temperature
  6. 6
    Sonstigethe solution was continuously reacted for 8 hours
  7. 7
    Extraktionthe solution was extracted by ether (30 mL) and deionized water (50 mL)
  8. 8
    SonstigeAn organic phase was collected
  9. 9
    SonstigeAfter removal of ether by a rotary concentrator
  10. 10
    workup.DISTILLATIONthe organic phase was purified by reduced-pressure distillation
  11. 11
    Sonstigeto form a transparent colorless oily product (21, 1.83 g, 78%)

Vorschrift

2.5 M of n-BuLi (2.1 mL/hexane, 5.32 mmol) was added to 4-bromobiphenyl (1.24 g, 5.32 mmol/THF (20 mL)) and reacted at −78° C. for 40 minutes under a dry and anaerobic operation condition to form a solution. SnBu3Cl (1.65 mL, 5.85 mmol) was then added to the solution and reacted at −78° C. for 1 hour. After returning to room temperature, the solution was continuously reacted for 8 hours. After the reaction was completed, the solution was extracted by ether (30 mL) and deionized water (50 mL). An organic phase was collected. After removal of ether by a rotary concentrator, the organic phase was purified by reduced-pressure distillation to form a transparent colorless oily product (21, 1.83 g, 78%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08759543B2uspto-grants-2014_06