Reaktion #742984
ord-8d8961b4498f45c493c8ac48ba937f36
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturcooled in an ice-bath (above f.p)
- 2Sonstigeto come to rt
- 3SonstigeReaction mixture
- 4Temperaturwas cooled
- 5FiltrationThe resulting yellow solid was filtered
- 6Waschenwashed with ice-water
- 7Sonstigedried
Vorschrift
Fuming nitric acid (83.3 mL) (>90%) was added slowly to a solution of 2,6-dimethyl bromobenzene (27.9 g, 150 mmol) in acetric acid (167 mL) and cooled in an ice-bath (above f.p). The mix was allowed to come to rt and later heated at 80° C. for 2 h. (HPLC showed no SM). Reaction mixture was cooled and poured into ice-water with stirring. The resulting yellow solid was filtered, washed with ice-water and dried to give 28.7 g of an yellow solid which was used as such in the next step.