A facile method for the synthesis of 2,3,3＇,4＇-biphenyltetracarboxylic dianhydride（a-BPDA） was reported,which comprises the steps of the dehalogenative coupling of dimethyl 4-chlorophthalate（4-DMCP） and dimethyl...A facile method for the synthesis of 2,3,3＇,4＇-biphenyltetracarboxylic dianhydride（a-BPDA） was reported,which comprises the steps of the dehalogenative coupling of dimethyl 4-chlorophthalate（4-DMCP） and dimethyl 3-chlorophthalate（3-DMCP） catalyzed by low-cost（Ph 3 P） 2 NiCl 2,the hydrolysis of tetra-ester and the dehydration of tetra-acid.In contrast to the conventional methods,this method has the advantage of low cost,convenient manipulation,available condition,high purity and good overall yield.Moreover,the single crystal structure of a-BPDA was analyzed by X-ray diffraction method.The X-ray data suggest that a-BPDA is a rigid,non-coplanar and non-linear structure.It contains three crystallographically independent molecules,in which the dihedral angles of the two linked phenyl rings are 44.75（4）°,46.37（3）° and 42.32（3）°,respectively.The title molecule is governed by a stronger intermolecular interaction in contrast to van der Waals interaction because of the special positions of anhydride groups.展开更多
基金Supported by the Ministry of Education Project Combining the Industry and Teaching with Research of Guangdong Province,China(No.2011B090400062)
文摘A facile method for the synthesis of 2,3,3＇,4＇-biphenyltetracarboxylic dianhydride（a-BPDA） was reported,which comprises the steps of the dehalogenative coupling of dimethyl 4-chlorophthalate（4-DMCP） and dimethyl 3-chlorophthalate（3-DMCP） catalyzed by low-cost（Ph 3 P） 2 NiCl 2,the hydrolysis of tetra-ester and the dehydration of tetra-acid.In contrast to the conventional methods,this method has the advantage of low cost,convenient manipulation,available condition,high purity and good overall yield.Moreover,the single crystal structure of a-BPDA was analyzed by X-ray diffraction method.The X-ray data suggest that a-BPDA is a rigid,non-coplanar and non-linear structure.It contains three crystallographically independent molecules,in which the dihedral angles of the two linked phenyl rings are 44.75（4）°,46.37（3）° and 42.32（3）°,respectively.The title molecule is governed by a stronger intermolecular interaction in contrast to van der Waals interaction because of the special positions of anhydride groups.
