The process involves treating a mixture of hydrocyanic acid, acetonitrile and acrylonitrile with acetone in the presence of an alkali metal hydroxide catalyst. The reaction mixture is neutralised with a mineral acid and the acetonitrile is distilled off. The distilln. residue which consists of a binary methyl acrylonitrile-acetone cyanhydrin mixture is decomposed with conc sulphuric acid in the presence of CuSO4 or hydroquinone and the required product is isolated. Pref. the treatment of the starting material with acetone is carried out at 15-20 degrees C. - Advantages lies in high yields, economy and simplicity of process. Uses in prodn. of high-temp glass and of coating material for steel, wood etc.