Reaktion #702079

ord-f37fe9ffefe043118a43409330e1db9f

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAn iced-water bath was used
  2. 2
    Sonstigethe temperature between 25° and 30°
  3. 3
    workup.ADDITIONwas added in portions over 30 minutes
  4. 4
    workup.ADDITIONpoured into a 9.5 liter battery jar
  5. 5
    Sonstigeequipped with an efficient stirrer
  6. 6
    FiltrationThe resulting solid was filtered off
  7. 7
    Waschenwashed well with water

Vorschrift

A 12 liter resin pot equipped with an efficient mechanical stirrer and a thermometer was charged with 90% (sp. gr. 1.4826) nitric acid (3.6 liters). An iced-water bath was used to keep the temperature between 25° and 30° while 1,2,3-trichlorobenzene (1.89 kg, 10.4 mol) was added in portions over 30 minutes. The resulting mixture was stirred for 30 minutes and then poured into a 9.5 liter battery jar equipped with an efficient stirrer and containing about 5 kg of ice. The resulting solid was filtered off and washed well with water.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04146718uspto-grants-1979_03