反应详情

To a solution of 1-[1-(4-bromo-phenyl)-1-methyl-ethyl]-4-(toluene-4-sulfonyl)-piperazine (200 mg, 0.45 mmol) in DMF (3 mL) was added zinc cyanide (64.41 mg, 0.54 mmol) and tetrakis(triphenylphosphine)palladium(0) (52 mg, 0.045 mmol) and the reaction mixture degassed for 10 min under N2. The reaction mixture was then subjected to microwave irradiation for 30 min at 180° C., afterwhich time the reaction was diluted with 1:1 CH2Cl2/EtOAc (20 mL), washed with water (2×10 mL), passed through a phase separation cartridge and concentrated in vacuo. The crude residue was purified by reverse phase preparative HPLC-MS to afford 4-{1-methyl-1-[4-(toluene-4-sulfonyl)-piperazin-1-yl]-ethyl]-benzonitrile as a cream solid (70 mg, 47%).

1. customthe reaction mixture degassed for 10 min under N2
2. customirradiation for 30 min at 180° C.
3. additionafterwhich time the reaction was diluted with 1:1 CH2Cl2/EtOAc (20 mL)
4. washwashed with water (2×10 mL)
5. custompassed through a phase separation cartridge
6. concentrationconcentrated in vacuo
7. customThe crude residue was purified by reverse phase preparative HPLC-MS