2,3,6,7,10,11-hexabromobenzo[9,10]phenanthrene synthesis

Yield:82632-80-2 95%

Reaction Conditions:

with bromine;iron in nitrobenzene at 20 - 205; for 18.25 h;

Steps:

1.3 Example 1.3. Synthesis of 2,3,6,7,10,11-Hexabromotriphenylene (2)
To a solution of triphenylene (1, 1.07 g, 4.7 mmol) in nitrobenzene (40 mL) with iron powder (100 mg, 1.79 mmol) bromine (2.2 mL, 38.8 mmol) was slowly added over 15 minutes. The solution was then allowed to stand for 16 hours at room temperature. It was heated at 205 °C for 2 hours. The mixture was cooled to room temperature and mixed with diethyl ether (150 mL) and filtered. The crude white solid was washed by diethyl ether (3x30 mL) and acetone (3x10 mL). After drying in vacuo for 12 hours, 3.13 g of 2,3,6,7, 10,11-hexabromotriphenylene (yield 95%) was collected. The product was used directly without characterization due to low solubility.

References:

TRUSTEES OF DARTMOUTH COLLEGE;MIRICA, Katherine, A.;ZHAN, Xiaoping;MENDECKI, Lukasz;MENG, Zheng;KO, Michael WO2019/32804, 2019, A1 Location in patent:Paragraph 00173; 00174-00175

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