p-Bromoacetophenone → Tert-butyl 4-(4-acetylphenyl)piperazine-1-carboxylate

반응식

CC(=O)c1ccc(Br)cc1.CC(C)(C)OC(=O)N1CCNCC1>CC(=O)O.CC(=O)O.Cc1ccccc1.O=C([O-])[O-].[Cs+].[Cs+].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>CC(=O)c1ccc(N2CCN(C(=O)OC(C)(C)C)CC2)cc1

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온도: 120 °C

실험 절차

In a CEM MW vial, p-Bromoacetophenone (729 ml, 6.03 mmol),tert-Butyl 1-piperazinecarboxylate (1.684 g, 9.04 mmol),racemic-2,2'-Bis(diphenylphosphino)-1,1'-binaphthyl (0.375 g, 0.60 mmol),Palladium (II) acetate (0.135 g, 0.60 mmol),Cesium carbonate (3.93 g, 12.06 mmol) was taken in toluene (10 ml).The RM was subjected to MW power of 300W,temp 120°C for 45 minutes. The LCMS was checked showed the formation of required mass. Work-up: The RM was passed through hyflow bed and filtrate was evaporated and chrmatographed using Ethyl acetate hexane to obtain tert-butyl 4-(4-acetylphenyl)piperazine-1-carboxylate (0.963 g, 52.5 %).