Reaktion #53550

Reaktionsgleichung

nitric acid

2-bromo-m-xylene

→

2,6-dimethyl-3-nitrobromobenzene

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled in an ice bath (above freezing point)
2. 2
   Temperaturheated at 80° C. for 2 hours or until the reaction
3. 3
   TemperaturThe reaction mixture is cooled to room temperature
4. 4
   workup.STIRRINGwith stirring
5. 5
   SonstigeThe resulting yellow precipitates
6. 6
   Filtrationare collected by suction filtration and air
7. 7
   Sonstigedried

Vorschrift

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.

Quelle