反应详情

After dissolving (6-ethyl-3-pyridyl)methanol (2.25 g, 16.4 mmol) in toluene (25 ml), diphenylphosphoryl azide (4.2 ml, 19.6 mmol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (2.9 ml, 19.6 mmol) were added while stirring on ice, and the mixture was further stirred at room temperature for 18 hours. Water was added for treatment and extraction was performed with ethyl acetate. The extract was washed with brine and then dried over sodium sulfate and filtered. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (2.2 g) as a yellow oil. (84.5% yield)

1. additionwere added
2. stirringthe mixture was further stirred at room temperature for 18 hours
3. washThe extract was washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under reduced pressure
7. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)