反应详情

A solution of 1-methyl-4-(3-nitrophenyl)piperazine (EP0533267A) (1.0 g; 4.5 mmol) in glacial acetic acid (25 ml) was treated with bromine (0.23 ml; 1 equivalent). The reaction mixture was stirred at 75° overnight, then cooled, filtered, and the yellow sticky solid was partitioned between potassium carbonate (aq) and 2% methanol in dichloromethane. The organic phase was dried (Na2SO4) and evaporated under reduced pressure to leave the title compound (D26) as a viscous orange oil (928 mg, 68%) MH+=300/302.

1. temperaturecooled
2. filtrationfiltered
3. customthe yellow sticky solid was partitioned between potassium carbonate (aq) and 2% methanol in dichloromethane
4. dry with materialThe organic phase was dried (Na2SO4)
5. customevaporated under reduced pressure