反応 #3172

ord-84962d33083243bb8070accd1465b529

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the coupling reaction mixture
  2. 2
    温度was heated
  3. 3
    温度to reflux in an oil bath for 10 hours
  4. 4
    温度to being heated in an oil bath for 0.5 hour
  5. 5
    workup.STIRRINGwith periodically stirring)
  6. 6
    その他No further purification
  7. 7
    その他by recrystallization

実験手順

The same procedures set forth above in Example (1)(a) for synthesizing 3(3,4,5-trifluorophenyl)thiophene were followed, with the exception that 1-bromo-2,4-difluorobenzene was substituted for 1-bromo-3,4,5-trifluorobenzene as the 1-bromo-substituted fluorobenzene, and the coupling reaction mixture was heated to reflux in an oil bath for 10 hours with stirring at 80° C. (as opposed to being heated in an oil bath for 0.5 hour with periodically stirring). No further purification by recrystallization was required to obtain a 97 to 98% pure product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05733683uspto-grants-1998_03