반응 #420932

ord-78fd86b8e46e4ae797e11cd5c88aa4e8

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooling for 30 min
  2. 2
    workup.STIRRINGthe mixture was stirred at room temperature for 17 hr
  3. 3
    농축the mixture was concentrated under reduced pressure
  4. 4
    기타The residue was purified by silica gel column chromatography (ethyl acetate/methanol)

실험 절차

Under an argon atmosphere, to a solution of 2-[3-(benzyloxy)propyl]-3H-imidazo[4,5-b]pyridine (2 g) in DMF (40 mL) was added 60% sodium hydride (0.299 g), and the mixture was stirred under ice-cooling for 30 min. Then, dimethylsulfuric acid (0.75 mL) was added, and the mixture was stirred at room temperature for 17 hr. To the reaction mixture was added methanol (5 mL), and the mixture was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/methanol) to give the title compound (1.2 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08883788B2uspto-grants-2014_11