反应详情

8.5 g (0.1 mole) of cyano acetic acid are dissolved in 350 ml. of ethylether and cooled to 0° C. 20.1 g. (0.1 mole) of phosphorus pentachloride are added. The cooling is stopped and the temperature is slowly raised to room temperature. When the HCl evolution ceases the solvent is distilled off in vacuo. The residue containing the formed cyanoacetic acid chloride and phosphoroxychloride is taken up in 50 ml. of dichloromethane and 26 g. (0.1 mole) of pentachlorophenol and 11 ml. (0.1 mole) of N,N'-dimethylaniline are added dropwise in 300 ml. of dichloromethane.

1. distillationis distilled off in vacuo
2. additionThe residue containing the formed cyanoacetic acid chloride and phosphoroxychloride