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ChemicalBook CAS DataBase List (2-(4-vinylphenyl)ethene-1,1,2-triyl)tribenzene

(2-(4-vinylphenyl)ethene-1,1,2-triyl)tribenzene synthesis

11synthesis methods
-

Yield: 86%

Reaction Conditions:

with titanium tetrachloride;zinc in tetrahydrofuran at 0 - 60; for 6 h;Reagent/catalyst;Solvent;Temperature;

Steps:

1.2-2.2 Step 2: Preparation of [1-(4-vinylphenyl)-1,2,2-triphenyl]ethylene
Under stirring at room temperature, 600g of zinc powder and 8L of tetrahydrofuran were added to the 20L reaction kettle and stirred evenly.Further, the reaction liquid was cooled to 0 degrees, and 550 g of titanium tetrachloride was added dropwise thereto. After the dropping, the reaction solution was stirred and reacted for 2 hours.Furthermore, a solution of 560 g of the previous step intermediate (light yellow solid) and 540 g of benzophenone dissolved in 2 L of tetrahydrofuran was added dropwise to the reaction solution. After the dropping, the reaction solution was heated to 60 degrees and reacted for 6 hours, and the reaction was completed.Further, the reaction solution was cooled to room temperature, and then 5 L of 15% potassium carbonate aqueous solution was added to quench the reaction.Further, the reaction solution was subjected to pressure filtration to filter out the solids, the filtrate was collected, the filtrate was allowed to stand for layering, the organic phase was collected, and the aqueous phase was extracted twice with 3L of dichloromethane.Further, the organic phases are combined, and the solvent is recovered by distillation under normal pressure. The residue was recrystallized from toluene to obtain 832 g of a pale yellow solid powder product with a yield of 86%.Product HPLC purity: 98.7%.

References:

Suzhou Bailingwei Chaojingxi Materials Co., Ltd.;Long Tao;Chen Pizheng;Gu Yang;Zou Zenglong CN111533637, 2020, A Location in patent:Paragraph 0039; 0048-0057; 0059; 0068-0077

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