Reaktion #346272

ord-1ff2ed2186f145959a277f01e6c1d577

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux
  2. 2
    Temperaturunder reflux
  3. 3
    Sonstigethe methylene chloride phase was separated off
  4. 4
    Temperaturwithout cooling
  5. 5
    Waschenwashed three times while still hot with 3 × 200 ml of water
  6. 6
    SonstigeAfter the washing water had been carefully separated off
  7. 7
    workup.DISTILLATIONthe methylene chloride was distilled off
  8. 8
    Sonstigeleaving 89.9 g (98% of the

Vorschrift

68.6 g (0.5 mol) of 2-nitrotoluene were dissolved in 80 ml of methylene chloride and 38.6 g (0.6 mol) of 98% by weight nitric acid, followed by the addition under reflux with stirring over a period of 1 hour at boiling temperature of 40 g of 100% by weight sulphuric acid. After stirring for 2 hours under reflux, the methylene chloride phase was separated off without cooling and washed three times while still hot with 3 × 200 ml of water. After the washing water had been carefully separated off, the methylene chloride was distilled off, leaving 89.9 g (98% of the theoretical yield) of dinitrotoluene containing 99% of 2,4- and 2,6-dinitrotoluene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04036838uspto-grants-1977_07