반응 #43682

ord-c9b724ccf96a4746a1af2ce58abf5586

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed overnight under an argon atmosphere
  2. 2
    기타an insoluble material was removed by filtration
  3. 3
    세척The filtrate washed with 1 mol/L hydrochloric acid, water and brine successively
  4. 4
    건조dried over anhydrous magnesium sulfate
  5. 5
    기타the solvent was removed under reduced pressure
  6. 6
    기타The residue was purified by column chromatography on silica gel (eluent: n-hexane-n-hexane/ethyl acetate=5/1)

실험 절차

A mixture of 4-bromobenzo[b]thiophene (0.55 g), styrene (0.89 mL), triethylamine (1.81 mL), palladium(II) acetate (59 mg) and tris(2-methylphenyl)phosphine (0.16 g) in acetonitrile (10 mL) was refluxed overnight under an argon atmosphere. The reaction mixture was diluted with diethyl ether and an insoluble material was removed by filtration. The filtrate washed with 1 mol/L hydrochloric acid, water and brine successively, and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane-n-hexane/ethyl acetate=5/1) to give the title compound (0.56 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732596B2uspto-grants-2010_06