Reaktion #723547
ord-2266022b3c2b4c089ee2e65a2844c88c
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigeat 25-30° C
- 2Filtrationfiltered
- 3WaschenThe filter cake is washed (15 L water)
- 4workup.DISSOLUTIONdissolved in 58 L of ethyl acetate
- 5WaschenThe organic phase is washed with water, aqueous sodium bicarbonate solution, and aqueous sodium chloride solution
- 6TrocknenThe solution is dried over magnesium sulfate
- 7Einengenconcentrated
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.