Reaktion #60235

Reaktionsgleichung

sodium t-butoxide

2-bromo-7-iodo-9,9-dimethylfluorene

diphenylamine

N,N′-dimethylethylene-diamine

→

yellow solid

Ausbeute 69.9%

2-(N,N-diphenylamino)-7-bromo-9,9-dimethylfluorene

Ausbeute 69.9%

Lösungsmittel

xylene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONCharged under Ar atmosphere
2. 2
   Temperaturthe mixture was refluxed for 24 hours
3. 3
   Temperaturunder heating
4. 4
   Extraktionthe mixture was extracted with toluene
5. 5
   Filtrationthe insoluble matter was filtered
6. 6
   EinengenThe filtrate was concentrated

Vorschrift

Charged under Ar atmosphere were 2-bromo-7-iodo-9,9-dimethylfluorene 20.0 g, diphenylamine 8.46 g, copper iodide 0.476 g, N,N′-dimethylethylene-diamine 0.441 g, sodium t-butoxide 7.21 g and xylene 50 ml, and the mixture was refluxed for 24 hours under heating. After cooled down to room temperature, the mixture was extracted with toluene, and the insoluble matter was filtered. The filtrate was concentrated, and then the concentrate was refined by silica gel chromatography to obtain 15.4 g of a yellow solid matter of 2-(N,N-diphenylamino)-7-bromo-9,9-dimethylfluorene.

Quelle