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ChemicalBook CAS DataBase List 4,4'-DIBROMOOCTAFLUOROBIPHENYL
10386-84-2

4,4'-DIBROMOOCTAFLUOROBIPHENYL synthesis

3synthesis methods
-

Yield:10386-84-2 92.3%

Reaction Conditions:

Stage #1:1,4-dibromotetrafluorobenzene with magnesium;ethylene dibromide in tetrahydrofuran at 20; for 6.25 h;Inert atmosphere;
Stage #2: with (4-bromophenyl)magnesium bromide;copper(l) chloride in tetrahydrofuran at 10 - 15; for 3 h;Reagent/catalyst;Solvent;Temperature;

Steps:

1-7 Example 7
Add 5.35 g of fresh magnesium chips, 60 g of anhydrous tetrahydrofuran, nitrogen protection, stirring at room temperature into a 250 ml reaction flask, add 0.2 g of dibromoethane with a syringe, stir for 15 minutes, and slowly add 61.57 g of A mixed solution of 2,3,5,6-tetrafluoro-1,4-dibromobenzene and 60 grams of anhydrous tetrahydrofuran, after the dripping is completed, stir and react at room temperature for 6 hours to obtain 2,3,5,6-tetrafluoro-4-bromobenzene Base magnesium bromide solution, set aside.Take another 500 ml reaction flask, add 23.75 g cuprous chloride and 100 g anhydrous tetrahydrofuran, turn on the stirring, control the temperature of the system (10-15) , and add dropwise the prepared 2,3,5,6-tetrafluoro- After the addition of 4-bromophenyl magnesium bromide solution is completed, the reaction is stirred at (10-15)°C for 3 hours. The reaction solution was diluted to 150 g of 10percent hydrochloric acid solution, extracted twice with ethyl acetate, and the organic phases were combined, dried over anhydrous sodium sulfate and concentrated to remove the solvent. The residue was decolorized by activated carbon and recrystallized to obtain a white solid 42.08 Gram is 2,2',3,3',5,5',6,6'-octafluoro-4,4'-dibromobiphenyl, the yield is 92.3percent, and the purity is 99.3percent.

References:

Zhejiang Zhongxinfucai Co., Ltd.;Yuan Qiliang;Chen Haifeng;Xie Bowen;Xu Pengfei;Chen Yinhao;Wang Chao CN111393256, 2020, A Location in patent:Paragraph 0012; 0027-0047

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