تفاعل #60235

معادلة التفاعل

sodium t-butoxide

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

diphenylamine

N,N′-dimethylethylene-diamine

→

yellow solid

المردود 69.9%

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

المردود 69.9%

المذيبات

xylene

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONCharged under Ar atmosphere
2. 2
   درجة الحرارةthe mixture was refluxed for 24 hours
3. 3
   درجة الحرارةunder heating
4. 4
   استخلاصthe mixture was extracted with toluene
5. 5
   ترشيحthe insoluble matter was filtered
6. 6
   تركيزThe filtrate was concentrated

الإجراء التجريبي

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.

المصدر