The ketone-ester condensation of acetylferrocene (1) with methyl 4-alkoxy-3-bromobenzoates (2) afforded 1-ferrocenyl-3-(4-alkoxy-3-bromophenyl)-1,3-propanediones (3), which showed complicated resonance structures. The structures of 3 were characterized by elemental analysis, IR, and 1H NMR spectra. X-ray diffraction method was also used to determine the structure of compounds 1-ferrocenyl-3-(4-dodecyl- 3-bromophenyl)-1,3-propanedione (3c) and the crystal data belong to triclinic, P-1 space group with unit cell dimensions a＝0.8677(5) nm, b＝0.8791(5) nm, c＝2.1444(11) nm, α＝101.489(9)°, β＝94.784(10)°, γ＝102.522(9)°, V＝1.5511(14) nm3, Dc＝1.273 g•cm－3, μ＝0.005 mm－1, F(000)＝618, Z＝2, R1＝0.0597 and wR2＝0.1386.

Key words: ferrocene, bromo-substitution, X-ray diffracti, long-chained alkoxy, 1,3-propanedione