Nitric Acid → 2-Bromo-1,3-dimethyl-4-nitrobenzene

HRID 25272

Reaktionsgleichung

Reaktionsgleichung von HRID 25272
[N+:1]([O-:4])(O)=[O:2].[Br:5][C:6]1[C:11]([CH3:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH3:13]>C(O)(=O)C>[CH3:13][C:7]1[C:8]([N+:1]([O-:4])=[O:2])=[CH:9][CH:10]=[C:11]([CH3:12])[C:6]=1[Br:5]

Komponenten

4

Versuchsvorschrift

Fuming nitric acid (>90% yellow fuming HNO3) is slowly added to a solution of 2-bromo-m-xylene (20 g, 150 mmol) in acetic acid (100 ml) cooled in an ice bath (above freezing point). The resulting mixture is allowed to warm to room temperature, stirred for 1 hour, and heated at 80° C. for 2 hours or until the reaction is shown to be complete by GC/MS analysis following micro-scale base work-up. The reaction mixture is cooled to room temperature and poured into ice/water with stirring. The resulting yellow precipitates are collected by suction filtration and air dried to obtain 2,6-dimethyl-3-nitrobromobenzene.

Aufarbeitung

  1. temperaturecooled in an ice bath (above freezing point)
  2. temperatureheated at 80° C. for 2 hours or until the reaction
  3. temperatureThe reaction mixture is cooled to room temperature
  4. stirringwith stirring
  5. customThe resulting yellow precipitates
  6. filtrationare collected by suction filtration and air
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-be524cb8b1a6445599b71a2c69566762
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06858637B2

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