反应详情

温度

100 °C

A mixture of tert-butyl 4-(4-bromo-2-tert-butylphenyl)piperazine-1-carboxylate (Example 85, 3.0 g, 7.55 mmol), zinc cyanide (1.77 g, 15.1 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.88 g, 0.76 mmol) in DMF (30 mL) was stirred at 100° C. for 4 h under argon atmosphere. The reaction mixture was cooled to room temperature, poured into saturated NaHCO3 solution and extracted with ethyl acetate. The organic layer was washed with brine, dried over MgSO4, and the solvent was evaporated under reduced pressure to give the crude product. The product was purified by flash column chromatography (silica gel, n-hexane/ethyl acetate=95:5 to 80:20) to provide tert-butyl 4-(2-tert-butyl-4-cyanophenyl)piperazine-1-carboxylate (2.29 g, 88%) as a white powder.

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried over MgSO4
5. customthe solvent was evaporated under reduced pressure
6. customto give the crude product
7. customThe product was purified by flash column chromatography (silica gel, n-hexane/ethyl acetate=95:5 to 80:20)