Under argon protection, NiCl2-6H2O (0.05 mmol, 11.9 mg), dppf (0.06 mmol, 33.3 mg), Zn (0.2 mmol, 13.0 mg), DMAP (1.0 mmol, 122.2 mg), Zn(CN)2 (0.8 mmol, 93.9 mg), o-chloroacetophenone (1.0 mmol, 140.6 mg) and acetonitrile (5.0 mL) were added to a 25.0 mL sealed tube. The reaction mixture was placed in an oil bath at 60°C for 6 hours. After completion of the reaction, it was cooled to room temperature and the reaction solution was filtered directly through a short silica gel column and washed with dichloromethane. The filtrate was concentrated and purified by silica gel column chromatography (wet sampling was used to avoid sample loss). The eluent ratio was petroleum ether/ethyl acetate=20:1, and 117.2 mg of 2-acetylbenzonitrile was obtained as a white solid with 88% yield, and the 1H NMR showed a purity of more than 98%.
