Dimethylamine → 2-(4-fluorophenyl)-2-(N,N-dimethylamino)acetonitrile

Beteiligte Stoffe

Reaktionsschritte

Into a 1 l four-necked flask equipped with a thermometer, a stirrer and a dropping funnel, 144.5 g (1.6 mol) of a 50.7% dimethylamine aqueous solution and 118.5 g of water were charged, and 159.4 g (0.38 mol) of a 25% of sulfuric acid aqueous solution was dropwise added over a period of 15 minutes at a temperature of not higher than 20° C. with stirring. Then, 67.4 g (1.38 mol) of sodium cyanide was introduced. Then, 155.1 g (1.25 mol) of 4-fluorobenzaldehyde was dropwise added over a period of 20 minutes at from 20 to 30° C. Thereafter, the reaction was carried out at 50° C. for 4 hours. After completion of the reaction, the reaction mixture was subjected to liquid separation. The organic layer was separated and washed with 500 ml of water of 50° C. to obtain 222.8 g (yield: 98.4%) of the desired compound having a purity of 98.4% (by GC analysis).

Herkunft & Nachweise