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).