反应详情

To a RB flask equipped with magnetic stirring bar, reflux condenser, N2 inlet line with bubbler was added phenanthro[1,2-b]furan-2-methanol (14A, 5.84 g, 23.5 mmol), barium manganate (Aldrich, 12.06 g, 47 mmol) and dry CH2Cl2 (400 mL). The mixture was refluxed for 6 h, filtered and the resulting dark yellow solution filtered through a small plug of SiO2 to remove inorganic salts and polar baseline material. The solvent was then removed by rotary evaporation and the crude material recrystallized using CH2Cl2 /hexane to give after drying 5.17 g (91% yield) of phenanthro[1,2-b]furan-2-carbaldehyde, mp 169° , (C,H).

1. customTo a RB flask equipped with magnetic stirring bar
2. temperaturereflux condenser, N2 inlet line with bubbler
3. temperatureThe mixture was refluxed for 6 h
4. filtrationfiltered
5. filtrationthe resulting dark yellow solution filtered through a small plug of SiO2
6. customto remove inorganic salts and polar baseline material
7. customThe solvent was then removed by rotary evaporation
8. customthe crude material recrystallized
9. customto give