1,2,4-Trichlorobenzene → 2,4,5-Trichloronitrobenzene

HRID 67806

Reaktionsgleichung

Reaktionsgleichung von HRID 67806
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[Cl:9].[N+:10]([O-])([OH:12])=[O:11]>O>[Cl:1][C:2]1[CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]([Cl:8])=[CH:4][C:3]=1[Cl:9]

Komponenten

4

Edukt 2

HCID 131,2,4-TrichlorobenzeneHCID 944Nitric Acid

Produkt 1

HCID 69832,4,5-Trichloronitrobenzene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

2723 gm (15.0 mols) of 1,2,4-trichlorobenzene were added to 7350 gm (105 mols) of 90% fuming nitric acid at 40° C. over a 3 hour period. The reaction mixture was held at 40° C. for one hour and worked up by the addition of 3700 ml of H2O while maintaining a temperature of 55°-60° C., and separating the waste acid. Two additional washes with 2000 ml of hot (55° C.) water and 1000 ml of 10% sodium bicarbonate solution followed by a phase separation gave 3316 gm (14.64 mols) of crude 1,2,4-trichloro-5-nitrobenzene. An additional 33 gm product was recovered from the waste acid when cooled and filtered.

Aufarbeitung

  1. customat 40° C.
  2. customover a 3 hour
  3. temperaturewhile maintaining a temperature of 55°-60° C.
  4. customseparating the waste acid
  5. customTwo additional washes with 2000 ml of hot (55° C.) water and 1000 ml of 10% sodium bicarbonate solution followed by a phase separation

Quellen und Nachweise

ORD-Eintrag
ord-e53549ce01a2493a96142624339f6386
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04346248

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