Sodium Sulfate → 4-(Methylthio)benzonitrile

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

With stirring (20 rpm), a turbine dryer is charged at room temperature with 4000 parts by weight of anhydrous sodium sulfate, 950 parts by weight of 4-(methylthio)benzaldehyde and 538.4 parts by weight of hydroxylammonium sulfate. Following evacuation to 25 mbar, the mixture is heated to 80° C. and stirred at this temperature for 3 hours. It is subsequently heated at 130° C. and held for 30 minutes at the same pressure. A total of about 240 parts by weight of water are removed by distillation altogether. The distillation of the nitrile is initiated and controlled by reduction of the pressure to 5 mbar and subsequent raising of the jacket temperature to 150° C. 708 parts by weight of 4-(methylthio)benzonitrile are obtained with a purity of over 98% (TLC), and also 18 parts by weight of a mixed fraction essentially consisting of 4-(methylthio)benzonitrile and 4-(methylthio)benzaldehyde. The collected 4-(methylthio)benzonitrile has a melting point of 61°-63° C.

Herkunft & Nachweise