反应详情

The round bottom flask was heated then allow to cool to room temperature under argon. Add Pd2(dba)3 (1.39 g, 1.52 mmoles, 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 mmoles) or 2-chlorotoluene (39 mL, 332.1 mmoles), lithium amide (3.47 g, 151.1 mmol, 45 mol %), sodium t-butoxide 29.5 g, 297.7 mmoles, 90 mol %), then toluene (150 mL). Heat at 80° C. under argon overnight. Let cool to room temperature. Diluted with diethyl ether then filtered through a pad of celite. Concentrated the resulting filtrate in vacuo. Used in the next reaction without purification. Purified the resulting residue by column chromatography with hexane to give 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. temperatureHeat at 80° C. under argon overnight
3. temperatureLet cool to room temperature
4. filtrationthen filtered through a pad of celite
5. concentrationConcentrated the resulting filtrate in vacuo
6. customUsed in the next reaction
7. customwithout purification
8. customPurified the resulting residue by column chromatography with hexane