반응 #157730

ord-c28d027628f646698aaa0af849896fb1

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=90:1→0:100)

실험 절차

Potassium carbonate (12 g) and 4-methoxybenzyl chloride (8.8 mL) were added to a solution of 2-bromo-6-iodopyridin-3-ol (12 g) in N,N-dimethylformamide (130 mL), and the mixture was stirred at room temperature for six hours. 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=90:1→0:100) to give 2-bromo-6-iodo-3-[(4-methoxybenzyl)oxy]pyridine as a colorless powder (18 g, 100%).

출처

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