Reaktion #723547

ord-2266022b3c2b4c089ee2e65a2844c88c

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat 25-30° C
  2. 2
    Filtrationfiltered
  3. 3
    WaschenThe filter cake is washed (15 L water)
  4. 4
    workup.DISSOLUTIONdissolved in 58 L of ethyl acetate
  5. 5
    WaschenThe organic phase is washed with water, aqueous sodium bicarbonate solution, and aqueous sodium chloride solution
  6. 6
    TrocknenThe solution is dried over magnesium sulfate
  7. 7
    Einengenconcentrated

Vorschrift

A mixture of 9.0 kg of 1,2,3-trichlorobenzene in 13.32 L of concentrated sulfuric acid is acid by drops to a solution of 4.13 L of 70% nitric acid and 4.13 L of concentrated sulfuric acid at 25-30° C. The slurry is stirred for 1.5-2 hours, then poured over 35 kg of ice and filtered. The filter cake is washed (15 L water) and then dissolved in 58 L of ethyl acetate. The organic phase is washed with water, aqueous sodium bicarbonate solution, and aqueous sodium chloride solution. The solution is dried over magnesium sulfate and concentrated to give the title product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06194420B1uspto-grants-2001_02