反応 #3785

ord-a4ed8d077a2e4b55a7f88a3b17be86f8

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the reaction mixture was refluxed for two hours
  2. 2
    濃縮It was then concentrated under reduced pressures
  3. 3
    抽出extracted with diethylether
  4. 4
    洗浄rinsed with water
  5. 5
    その他With the diethylether removed under reduced pressures
  6. 6
    その他the product was purified by alumina column chromatogram

実験手順

1,2-Bis(5-bromo-2-methyl-3-thienyl)hexafluorocyclopentene (1.0 g 0.002 mol) was dissolved in dimethoxyethane (50 ml), and palladium tetra(triphenylphosphine) (120 mg) was added to the mixture which was stirred for 5 minutes under argon atmosphere. With 4-methyl-2-thienyl boric acid (852 mg, 0.006 mol) and an aqueous solution of potassium carbonate (0.1 mol dm-3, 10 ml) were added, the reaction mixture was refluxed for two hours. It was then concentrated under reduced pressures, extracted with diethylether and rinsed with water. With the diethylether removed under reduced pressures, the product was purified by alumina column chromatogram to give 1,2-bis[2-methyl-5-(4-methyl-2-thienyl)-3-thienyl]hexafluorocyclopentene (447 mg, 0.0008 mol).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05734065uspto-grants-1998_03