Sodium Sulfate → 4-tert-Butylbenzonitrile

HRID 53402

Reaktionsgleichung

Reaktionsgleichung von HRID 53402
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]

Komponenten

5

Edukt 3

HCID 24436Sodium SulfateHCID 24846Hydroxylamine sulfateHCID 703244-tert-Butylbenzaldehyde

Produkt 1

HCID 778834-tert-Butylbenzonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

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.

Aufarbeitung

  1. stirringstirred at this temperature for 2 hours
  2. customare removed by distillation
  3. distillationThe distillation of the nitrile
  4. temperatureraising of the jacket temperature to 170° C

Quellen und Nachweise

ORD-Eintrag
ord-519708dec3b74f5589276c5767db7ef4
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05618965

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