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ChemicalBook CAS DataBase List 2-bromo-7-N,N’-diphenylamino-9,9’-dimethyl-9H-fluorene

2-bromo-7-N,N’-diphenylamino-9,9’-dimethyl-9H-fluorene synthesis

4synthesis methods
319906-45-1 Synthesis
7-Bromo-2-iodo-9,9-dimethyl-9H-fluorene

319906-45-1
113 suppliers
$16.00/5g

2-bromo-7-N,N’-diphenylamino-9,9’-dimethyl-9H-fluorene

302579-16-4
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Yield: 89.4%

Reaction Conditions:

with 18-crown-6 ether;copper;potassium carbonate in 1,2-dichloro-benzene for 4 h;Inert atmosphere;

Steps:

1.1
In a 500-liter three-bottle, with electric stirring, Ar gas protection, 16.9 g of diphenylamine (molecular weight 169, 0.10 mol), 44 g (molecular weight 398, 0 • 1 lmol) of 2-bromo-7-iodo-9,9-dimethylfluorene, Copper powder 15 g (molecular weight 64,0.234 mol), Potassium carbonate 41.4 g (molecular weight 138, 0.3 mol), 18-crown-6 with 6,13 g (molecular weight 264, 023 mol) Add 300 ml of solvent to o-dichlorobenzene. The mixture was stirred for 4 hours and the reaction was monitored with TLC. After completion of the reaction, the mixture was naturally stirred to room temperature and the solvent was distilled off. The solid mixture was chromatographed on silica gel to give 40.3 g of a slightly yellow bromide intermediate, a molecular weight of 439, a purity of 97.5% and a yield of 89.4%.

References:

Beijing Dingcai Technology Co., Ltd.;Li Yinkui;Li Yanrui;Fan Hongtao CN104672230, 2017, B Location in patent:Paragraph 0055; 0056; 0057