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ChemicalBook CAS DataBase List 2,3,3,4-biphenyl tetracarboxylic dianhydride

2,3,3,4-biphenyl tetracarboxylic dianhydride synthesis

9synthesis methods
The preparation of 2,3,3',4'-biphenyl tetracarboxylic dianhydride is as follows:In a 1000 ml three-necked flask, 18.3 g (0.1 mol) of 4-chlorophthalic anhydride and 18.3 g (0.1 mol) were added 3-chlorophthalic anhydride, 300 g of anisole as solvent, 0.13 g (0.001 mol) of nickel chloride as a catalyst, 0.198 g (0.001 mol) of C-1 as a catalyst ligand, and 0.03 g (0.0003 mol) of sodium bromide as a catalyst Auxiliary, 13 g (0.2 mol) of zinc powder was used as a reducing agent, and the reaction was stirred at 30 ° C for 8 hours under a nitrogen atmosphere. The reaction solution was filtered to remove insoluble solids in the reaction liquid. 300 g of methanol was added to the filtration mother liquor, and the product was precipitated, filtered, and dried to obtain 25.8 g of the product 2,3,3',4'-biphenyltetracarboxylic dianhydride, yield 87.7%. 

36978-41-3.png

36978-40-2 Synthesis
1,1'-Biphenyl-2,3,3',4'-tetracarboxylic acid

36978-40-2
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Yield:36978-41-3 92.4%

Reaction Conditions:

with acetic anhydride in toluene at 100; for 4 h;Temperature;

Steps:

1.5

Step 5: Add 41.9g of 2,3,3',4'-biphenyltetracarboxylic acid200ml of toluene,Add 38.8g of acetic anhydride,Turn on stirring,The temperature is controlled at 100°C,Incubate the reaction for 4h,After crystallization, decolorization,secondary crystallization,After drying, 34.5 g of α-BPDA in white solid state was obtained.The yield of α-BPDA was calculated to be 92.4%,HPCL purity is 99.88%,

References:

CN114230540,2022,A Location in patent:Paragraph 0077; 0079; 0085

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