Reaktion #60236

Reaktionsgleichung

N,N′-dimethylethylenediamine

diphenylamine

4-bromoiodobenzene

→

white crystal

Ausbeute 70.2%

4-bromotriphenylamine

Ausbeute 70.2%

Lösungsmittel

xylene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 24 hours under argon atmosphere
2. 2
   Filtrationthe mixture was filtered
3. 3
   Sonstigeto remove an insoluble matter
4. 4
   Einengenthe filtrate was concentrated

Vorschrift

N,N′-dimethylethylenediamine 1.76 g was added to diphenylamine 16.9 g, 4-bromoiodobenzene 28.2 g sodium t-butoxide 14.4 g, copper powder 3.81 g and a xylene 100 ml solution, and the mixture was heated and refluxed for 24 hours under argon atmosphere. After cooled down to room temperature, the mixture was filtered to remove an insoluble matter, and the filtrate was concentrated. The residue was refined by silica gel chromatography to obtain 22.7 g of white crystal of 4-bromotriphenylamine.

Quelle