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ChemicalBook CAS DataBase List Tetrakis(p-broMophenyl)Methane

Tetrakis(p-broMophenyl)Methane synthesis

11synthesis methods
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Yield:105309-59-9 68.5%

Reaction Conditions:

Stage #1:1.4-dibromobenzene with n-butyllithium in tetrahydrofuran;hexane at -78; for 1 h;Inert atmosphere;
Stage #2:tetrachloromethane in tetrahydrofuran;hexane at 27; for 14 h;

Steps:

1 Synthesis of the first target compound of the formula:
A solution of n-butyllithium n-hexane (6.6 mL, 10.5 mmol) was added dropwise to a solution of 1,4-dibromobenzene (2.36 g, 10 mmol) THF (20 mL).The reaction was carried out at -78 ° C under an inert atmosphere of argon for 1 h.Then, carbon tetrachloride (1.05 mL, 5 mmol) was added to the reaction solution and the above conditions were maintained for 2 h.After that, it was slowly heated to room temperature of 27 ° C and stirred for 12 h.Finally, 30 mL of water was added to interrupt the reaction and extraction was carried out using chloroform.The obtained organic layer was purified by column chromatography to give the intermediate product TBrBen (2.15 g, yield 68.5%).Identification of intermediate products by mass spectrometry, the results are:

References:

Yangtze Normal University;Yang Yezi;Yao Chuang;Sun Changqing CN108752320, 2018, A Location in patent:Paragraph 0022; 0023; 0024; 0030

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