반응 #3785

ord-a4ed8d077a2e4b55a7f88a3b17be86f8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction mixture was refluxed for two hours
  2. 2
    농축It was then concentrated under reduced pressures
  3. 3
    추출extracted with diethylether
  4. 4
    세척rinsed with water
  5. 5
    기타With the diethylether removed under reduced pressures
  6. 6
    기타the product was purified by alumina column chromatogram

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05734065uspto-grants-1998_03