反応 #60235

反応方程式

sodium t-butoxide

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

diphenylamine

N,N′-dimethylethylene-diamine

→

yellow solid

収率 69.9%

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

収率 69.9%

溶媒

xylene

反応条件

後処理

1. 1
   workup.ADDITIONCharged under Ar atmosphere
2. 2
   温度the mixture was refluxed for 24 hours
3. 3
   温度under heating
4. 4
   抽出the mixture was extracted with toluene
5. 5
   ろ過the insoluble matter was filtered
6. 6
   濃縮The filtrate was concentrated

実験手順

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.

出典