反应详情

温度

80 °C

To a solution of N-Boc-piperazine (2.02 g, 11.0 mmol) in DMSO (20 mL) was added 2-fluoro-6-chlorobenzonitrile (1.55 g, 10 mmol) and potassium carbonate (1.52 g, 11 mmol). The mixture was stirred at 80° C. for about 48 hours. The mixture was cooled to r.t. and diluted with diethyl ether (200 mL). The solution was washed with 1N HCl (2×20 mL), H2O (3×20 mL) and brine (20 mL) and then dried over sodium sulfate and concentrated to a yellow oil. Purification by flash chromatography (4:1 hexanes/ethyl acetate) gave the title compound (2.5 g, 86%) as a colorless oil.

1. temperatureThe mixture was cooled to r.t.
2. washThe solution was washed with 1N HCl (2×20 mL), H2O (3×20 mL) and brine (20 mL)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated to a yellow oil
5. customPurification by flash chromatography (4:1 hexanes/ethyl acetate)