反应详情

To a solution of 2-dimethylaminomethyl-bromobenzene (588 mg, 2.75 mmol) and 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (560 mg, 2.56 mmol) in toluene (10 mL) and n-BuOH (3 mL), Cs2CO3 (2.50 g, 7.67 mmol) in H2O (5 mL) was added, followed by addition of Pd(Ph3P)4 (200 mg, 0.17 mmol, 6%). The mixture was then heated at reflux for 4 h. EtOAc and H2O were added. The organic layer was separated, filtered, dried over Na2SO4, concentrated in vacuo. The residue was purified by a silica gel flash column using 50% EtOAc/hexanes (containing 1% TEA) as eluent to give a solid (300 mg). MS 182.0 (M—Me2N).

1. temperatureThe mixture was then heated
2. temperatureat reflux for 4 h
3. customThe organic layer was separated
4. filtrationfiltered
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe residue was purified by a silica gel flash column