反应详情

温度

70 °C

In a first flask 0.135 g of palladium acetate (0.135 g, 0.602 mmol) and BINAP (2,2′-bis(diphenylphosphino)-1,1′-binaphthyl) (0.375 g) were suspended in 5 mL of toluene and stirred at 70° C. for 30 min. In a second flask, 2-bromo-1-methyl-4-nitrobenzene (1 g, 4.63 mmol), tert-butyl piperazine-1-carboxylate (1.12 g, 6.02 mmol and sodium tert-butoxide (1.068 g, 11.11 mmol) were added to 5 mL of toluene and stirred for 30 min. at 60° C. To this mixture was added the contents of the first flask, and stirring was continued for 3 h at 60° C. The solvent was evaporated, the residue purified via silica gel chromatography with dichloromethane-methanol (0 to 100%) to yield the title compound (0.145 g).

1. stirringstirred for 30 min. at 60° C
2. additionTo this mixture was added the contents of the first flask
3. stirringstirring
4. waitwas continued for 3 h at 60° C
5. customThe solvent was evaporated
6. customthe residue purified via silica gel chromatography with dichloromethane-methanol (0 to 100%)