反应详情

温度

80 °C

A mixture of N-phenylnaphthalen-2-amine (Compound 20) (5.0 g, 22.8 mmol), 4,4′-dibromobiphenyl (17.8 g, 57 mmol), Pd(dppf)Cl2 (0.73 g, 1 mmol) and sodium tert-butoxide (2.4 g, 25 mmol) in toluene (250 mL) was degassed and heated at 80° C. overnight. The whole was poured into ethyl acetate (250 mL), washed with brine, dried over Na2SO4, loaded on silica gel and purified by flash column (hexanes to hexanes/dichloromethane 9:1). The desired fraction was collected, and concentrated. The resulting solid was filtered, and washed with methanol to give a white solid (Compound 21) (6.15 g, in 60% yield).

1. customwas degassed
2. additionThe whole was poured into ethyl acetate (250 mL)
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. custompurified by flash column (hexanes to hexanes/dichloromethane 9:1)
6. customThe desired fraction was collected
7. concentrationconcentrated
8. filtrationThe resulting solid was filtered
9. washwashed with methanol