반응 #157731

ord-123f671109544a23a689988da1088225

반응 조건

온도
90°CELSIUS
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=95:5→70:30)

실험 절차

Sodium methoxide (11 g) was added to a solution of 2-bromo-6-iodo-3-[(4-methoxybenzyl)oxy]pyridine (17 g) in dimethyl sulfoxide (90 mL), and the mixture was stirred at 90° C. for three 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=95:5→70:30) to give 6-iodo-2-methoxy-3-[(4-methoxybenzyl)oxy]pyridine as a colorless powder (10 g, 71%).

출처

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