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A novel approach to the synthesis of 2,2′,3,3′-biphenyltetracarboxylic dianhydride is described. The target compound was prepared by a nickel-catalyzed coupling reaction of dimethy 3-chlorophthalate (3-DMCP) for 4h at 70–80°C, followed by subsequent hydrolysis of tetra-ester in acid solution and dehydration of tetra-acid, with overall yield of 68%. The structures of the products were characterized...