反应详情

The round-bottom flask was heated then allow to cool to room temperature under argon. Added Pd2(dba)3 (1.39 g, 1.52 mmol, 1.0 mol %) or Pd(dba)2 (1.38 g, 2.4 mmol, 1.4 mol %), 2-(di-tert-butylphosphino)biphenyl (1.09 g, 3.65 mmol, 2.4 mol %), 2-bromotoluene (40 mL, 332.1 mmol) or 2-chlorotoluene (39 mL, 332.1 mmol), lithium amide (3.47 g, 151.1 mmol, 45 mol %), sodium t-butoxide (29.5 g, 297.7 mmol, 90 mol %), followed by toluene (150 mL). The reaction mixture was heated at 80° C. under argon overnight, then allowed to cool to room temperature. Diluted with diethyl ether then filtered through a pad of Celite. Concentrated the resulting filtrate in vacuo. Used the crude material in the next reaction without purification. (Crude material can be purified by flash chromatography with hexane which gave the product as white crystals with a yellow tint (23.4 g, 118.6 mmol, 72% yield)).

1. temperatureThe round-bottom flask was heated
2. temperatureThe reaction mixture was heated at 80° C. under argon overnight
3. temperatureto cool to room temperature
4. filtrationthen filtered through a pad of Celite
5. concentrationConcentrated the resulting filtrate in vacuo
6. customin the next reaction
7. customwithout purification
8. custom(Crude material can be purified by flash chromatography with hexane which