反应详情

温度

125 °C

A mixture of 2-azabicyclo[2.2.2]octan-3-one (0.6 g, 4.8 mmol), iodo benzene (1.16 g, 5.76 mmol), Cs2CO3 (2.36 g, 7.20 mmol), xantphos (0.22 g, 0.38 mmol) and 1,4-dioxane (30 ml) was charged in a sealed tube and degassed with argon gas for 15 min. Tetrakis(triphenylphosphine)palladium (0) (0.22 g, 0.19 mmol) was added and degassed for another 15 min and heated at 125° C. for 3 h. The reaction mixture was filtered and concentrated under reduced pressure to afford the crude compound. This was purified by column chromatography over neutral alumina using 0.5% MeOH in CHCl3 as eluent to afford 600 mg (62%) of 2-phenyl-2-aza-bicyclo[2.2.2]octan-3-one as pale yellow solid.

1. additionwas charged in a sealed tube
2. customdegassed with argon gas for 15 min
3. customdegassed for another 15 min
4. filtrationThe reaction mixture was filtered
5. concentrationconcentrated under reduced pressure
6. customto afford the crude compound
7. customThis was purified by column chromatography over neutral alumina using 0.5% MeOH in CHCl3 as eluent