反应详情

Diphenanthren-9-ylamine (4.50 g, 12.18 mmol), 1,4-dibromobenzene (3.02 mL, 25.12 mmol), Pd2(dba)3 (307 mg, 0.355 mmol), tris-o-tolyphosphine (0.255 mL, 0.837 mmol), sodium tert-butoxide (3.2 g, 33.49 mmol) were put in a 250 mL two-neck flask and dissolved in toluene. The solution was refluxed and stirred for 12 hours. After completion of the reaction, the solution was extracted with DI water/methylenechloride and distilled under reduced pressure to remove the solvent. The resultant was columned with a solution of n-hexane and methylenechloride (7:1). The resultant was distilled under reduced pressure and re-crystallized such that the wax compound was obtained, (2.8 g, yield: 44%).

1. temperatureThe solution was refluxed
2. customAfter completion of the reaction
3. extractionthe solution was extracted with DI water/methylenechloride
4. distillationdistilled under reduced pressure
5. customto remove the solvent
6. distillationThe resultant was distilled under reduced pressure
7. customre-crystallized such that the wax compound
8. customwas obtained