反应详情

温度

80 °C

A mixture of 4-diphenylaminophenyl boronic acid (2.57 g, 8.9 mmol), 4-bromo-iodobenzene (5.03 g, 17.8 mmol), Pd(PPh3)4 (0.58 g, 0.5 mmol) and K2CO3 (3.0 g, 22 mmol) in dioxane/water (80 mL/15 mL) was degassed and heated at about 80° C. for about 20 hours. The whole was mixed with water/dichloromethane, the organic phase was collected and washed with brine, dried over Na2SO4, loaded on silica gel, and purified by flash column (hexanes to hexanes/dichloromethane 30:1). The desired fraction was collected, and concentrated to give a white solid (Compound 12), which was filtered and washed with methanol (2.70 g, in 76% yield).

1. customwas degassed
2. additionThe whole was mixed with water/dichloromethane
3. customthe organic phase was collected
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. custompurified by flash column (hexanes to hexanes/dichloromethane 30:1)
7. customThe desired fraction was collected
8. concentrationconcentrated