반응 #157763

ord-89f6114bf4d848c3aab847590a690aff

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출followed by extraction with ethyl acetate
  2. 2
    세척The organic layer was washed with brine
  3. 3
    건조dried over anhydrous magnesium sulfate
  4. 4
    여과filtered
  5. 5
    기타The solvent was then evaporated under reduced pressure
  6. 6
    기타The residue was purified by silica gel column chromatography (hexane:ethyl acetate=50:1→20:1)

실험 절차

Potassium carbonate (4.1 g) and (3-bromopropoxy)-tert-butyldimethylsilane (4.1 g) were added to a solution of 4-bromothiophenol (3.0 g) in N,N-dimethylformamide, and the mixture was stirred at room temperature overnight. The reaction solution was poured into water, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=50:1→20:1) to give the title compound as a colorless oil (5.5 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822503B2uspto-grants-2014_09