Diethyl Vinylphosphonate

Experimental procedure¹⁾: to a dry flask is charged with amide (0.35 mmol), PdCl₂(PhCN)₂ (0.017 mmol), and CuCl (0.035 mmol). The reaction vessel is charged with oxygen followed by the addition of chlorobenzene (2 mL) and tetraethyl methylenediphosphonate (TEMDP, 0.035 mmol). The reaction mixture is stirred at 70 °C for 1 min and then diethyl vinylphosphonate (1.05 mmol) is added. The reaction mixture is stirred at 70 °C for 48 h under oxygen atmosphere. After the reaction is over, the solvent is evaporated under reduced pressure and the crude residue is purified by flash column chromatograph.