反应详情

温度

85 °C

Add 1-iodo-2,4,6-trichlorobenzene (1500 mg, 4.88 mmol), zinc cyanide (345 mg, 2.94 mmol) and tetrakis(triphenylphosphine)palladium(0) (282 mg, 0.244 mmol) to anhydrous DMF (30 mL). Heat to 85° C. overnight. Cool to room temperature, dilute with toluene, wash with 2 N ammonium hydroxide (3×) and saturated aqueous sodium chloride and concentrate. Purify by silica gel chromatography, eluting with hexanes/dichloromethane to give 2,4,6-trichlorobenzonitrile (850 mg, 84%): 1H NMR (400 MHz, CDCl3) δ 7.76 (s, 1H), 7.65 (s, 1H).

1. temperatureCool to room temperature
2. washwash with 2 N ammonium hydroxide (3×) and saturated aqueous sodium chloride
3. concentrationconcentrate
4. customPurify by silica gel chromatography
5. washeluting with hexanes/dichloromethane