反应详情

温度

80 °C

A mixture of 2,7-dibromo-9,9-dimethyl-9H-fluorene (31.64 g, 89.87 mmol), ditolylamine (8.865 g, 44.9 mmol), Pd(dppf)Cl2 (1.644 g, 2.25 mmol) and sodium tert-butoxide (10.796 g, 112.3 mmol) in toluene 400 mL was degassed and heated at about 80° C. overnight. The resulting mixture was poured into ethyl acetate (500 mL). After the precipitate was filtered off, the solution was washed with water and brine, dried over Na2SO4, loaded on silica gel and purified by flash column (hexane to hexanes/dichloromethane 99:1 to 95:5 gradients). After removal of solvent and recrystallization in dichloromethane/hexanes, a white solid (Compound 32) was obtained (14.0169 g, in 66.6% yield).

1. customwas degassed
2. additionThe resulting mixture was poured into ethyl acetate (500 mL)
3. filtrationAfter the precipitate was filtered off
4. washthe solution was washed with water and brine
5. dry with materialdried over Na2SO4
6. custompurified by flash column (hexane to hexanes/dichloromethane 99:1 to 95:5 gradients)
7. customAfter removal of solvent and recrystallization in dichloromethane/hexanes