Diferrocenylmethanol was treated with BF₃•OEt₂ in CH₂Cl₂ to generate the diferrocenylmethyl carbocation. Without separation from the reaction mixture, the ion was reacted with ethyl acetoacetate to afford the ethyl α-diferrocenylmethylacetate in fairly high yield which was recrystallized from benzene to provide sin-gle crystal. By X-ray single crystal diffraction determination, it was found that the crystal belongs to triclinic system with P , a＝0.82554(8) nm, b＝0.96962(10) nm, c＝1.46662(14) nm, α＝105.562(2)°, β＝90.771(2)°, γ＝96.727(2)°, V＝1.2191(19) nm³, D_c＝1.516 g•cm^－3, μ＝1.320 mm^－1, F(000)＝532 and Z＝2.

Key words: ethyl α-diferrocenylmethylacetate, crystal structure, ethyl acetoacetate, reaction, diferrocenylmethylcarbonium