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Synthesis of the third-order nonlinear materials: bis (l,4-dihydroxynaphthalene)tetrathiafulvalene and bis (1,4-dialkoxylnaphthalene) tetrathiafulvalene has been achieved in four steps, starting from 2,3-dichloro-l,4-naphthaquinone. The matcrials exhibit larger third-order nonlinear optical susceptibilities X(3).