Sodium Sulfate → 4-tert-Butylbenzonitrile

反応式

S([O-])([O-])(=O)=O.[Na+].[Na+].[C:8]([C:12]1[CH:19]=[CH:18][C:15]([CH:16]=O)=[CH:14][CH:13]=1)([CH3:11])([CH3:10])[CH3:9].S([O-])([O-])(=O)=O.O[NH3+:26].O[NH3+]>O>[C:8]([C:12]1[CH:19]=[CH:18][C:15]([C:16]#[N:26])=[CH:14][CH:13]=1)([CH3:11])([CH3:10])[CH3:9]

参加物

反応条件

温度: 100 °C

実験手順

With stirring (20 rpm), a turbine dryer is charged at room temperature with 1800 parts by weight of anhydrous sodium sulfate, 365 parts by weight of 4-tert-butylbenzaldehyde and 194 parts by weight of hydroxylammonium sulfate. Following evacuation to 25 mbar, the mixture is heated to 100° C. and stirred at this temperature for 2 hours. It is subsequently heated at 125° C. for 40 minutes, during which about 82 parts by weight of water are removed by distillation. The distillation of the nitrile is then initiated and controlled by successive reduction of the pressure to 10 mbar and raising of the jacket temperature to 170° C. 300 parts by weight of 4-tert-butylbenzonitrile are obtained with an outstanding purity of ~98-99% (HPLC), along with 18 parts by weight of a less pure fraction.