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The present invention pertains to a cost-efficient method for prepn. of di-substituted fluorenes in high yield. For example, diphenylmethane was reacted with tert-Bu chloride for 4,4'-di-tert-butyldiphenylmethane, which was further treated with bromine for 2,2'-dibromo-4,4'-di-tert-butyldiphenylmethane. 2,2'-Dibromo-4,4'-di-tert-butyldiphenylmethane prepd. above was treated with zinc dust in presence of tetraethylammonium iodide and a catalyst of NiBr2(DME) with a ligand of s-trans-N,N'-di-tert-butylethanediimine (prepn. given) in THF under dry nitrogen atm. with refluxing to give 3,6-di-tert-butylfluorene as a final product. Advantageously, the title process avoided using expensive and hazardous materials in prepn. of substituted fluorenes, and hence, is safe and cost efficient.