反应详情

A mixture of 2-(R)-methylpiperazine (0.124 g, 1.1 mmol), tris(dibenzylideneacetone)dipalladium(0) (49 mg, 0.05 mmol), rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (69 mg, 0.10 mmol) and sodium tert-butoxide (0.148 g, 1.5 mmol) were stirred in toluene (50 mL) under nitrogen for 15 min to give a blood red solution. 5-Bromo-1,2-dihydroacenaphthylene (0.256 g, 1.1 mmol) was added, the solution stirred under nitrogen and heated at reflux for 3 h. The mixture was cooled, diluted with dichloromethane and filtered through celite. The organic phase was washed with water, dried (MgSO4), filtered and evaporated in vacuo. The crude product was taken forward to the next step without further purification.

1. customto give a blood red solution
2. temperatureheated
3. temperatureat reflux for 3 h
4. temperatureThe mixture was cooled
5. filtrationfiltered through celite
6. washThe organic phase was washed with water
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customevaporated in vacuo
10. customThe crude product was taken forward to the next step without further purification