To a solution of 312 g. (3 moles) of sodium bisulfite in 750 ml. of water in a 3-l. beaker is added 225 ml. of a 37–40% formaldehyde solution, and the mixture is warmed to 60°. After cooling to 35°, 219 g. (309 ml., 3 moles) of diethylamine is added with hand stirring, and the mixture is allowed to stand for 2 hours. The beaker containing the reaction mixture is placed under a good hood, and to it is added a solution of 147 g. (3 moles) of sodium cyanide dissolved in 400 ml. of water with efficient stirring so that the two layers are thoroughly mixed. After 1.5 hours the upper nitrile layer is separated and dried over 25 g. of Drierite; it weighs 299–309 g. (90–92%). The crude product is purified by distillation; the portion boiling at 61–63°/14 mm., n²⁵D 1.4230, amounts to 298–302 g. (88–90%) (Note 1).