Реакция #60235

Уравнение реакции

sodium t-butoxide

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

diphenylamine

N,N′-dimethylethylene-diamine

→

yellow solid

Выход 69.9%

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

Выход 69.9%

Растворители

xylene

Условия реакции

Обработка

1. 1
   workup.ADDITIONCharged under Ar atmosphere
2. 2
   Температураthe mixture was refluxed for 24 hours
3. 3
   Температураunder heating
4. 4
   Экстракцияthe mixture was extracted with toluene
5. 5
   Фильтрацияthe insoluble matter was filtered
6. 6
   КонцентрированиеThe filtrate was concentrated

Методика

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.

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