반응 #164981

ord-76c644397f444352bb4e0c7420741d8f

용매

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출was then extracted with ethyl acetate
  2. 2
    세척The organic layer was washed with saturated aqueous sodium chloride
  3. 3
    기타the solvent was evaporated under a reduced pressure
  4. 4
    기타The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1)

실험 절차

To a mixture of 1,4-benzenedimethanol (5.5 g, 40 mmol), 2-fluoropyridine (1.3 g, 13 mmol) and N,N-dimethylformamide (15 mL) was added sodium hydride (1.4 g, 40 mmol, 66% in oil) at 0° C., which was stirred for 20 minutes at room temperature and for 1 hour at 70° C. Water was added to the reaction mixture, which was then extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1) to obtain the title compound (1.9 g, 66%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08841327B2uspto-grants-2014_09