反応 #3786

ord-197bcc85a93f490aae992086e3528101

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 5-(5-trimethylsilyl-2-thienyl)-2-thienyl boric acid (1.4 g, 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{5-trimethylsilyl-2-thienyl)-2-thienyl}-3-thienyl]hexafluorocyclopentene (550 mg, 0.0007 mol).

出典

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