反应详情

To a solution of 2-(4-methylsulfonylphenyl)-1-phenylazulene (0.20 g) in 1, 2-dichloroethane (20.0 ml) was added 1-fluoropyridinium triflate (0.28 g), and the reaction mixture was heated under reflux for 30 min. The mixture was poured into ice-water, and extracted with CHCl3. The combined CHCl3 extracts were washed with water and brine, dried over Na2 SO4, and concentrated. The crude product was purified by SiO2 column chromatography (benzenee/EtOAc, 20:1) to give the title compound (0.10 g) as green crystals; mp 120°-122° C.

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 30 min
3. extractionextracted with CHCl3
4. washThe combined CHCl3 extracts were washed with water and brine
5. customdried over Na2 SO4
6. concentrationconcentrated
7. customThe crude product was purified by SiO2 column chromatography (benzenee/EtOAc, 20:1)