반응 #164981
ord-76c644397f444352bb4e0c7420741d8f
반응 방정식
용매
반응 조건
온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1추출was then extracted with ethyl acetate
- 2세척The organic layer was washed with saturated aqueous sodium chloride
- 3기타the solvent was evaporated under a reduced pressure
- 4기타The 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%).