Abstract: A novel method of synthesis of bis(methylcyclopentadienyl) titanium dichloride(Ⅰ) by reacting methylcyclopentadiene with titanium tetrachloride in the presence of diethylamine in tetrahydrofuran has been developed. Bis(methylcyclopentadienyl) titanium diphenoxide(Ⅱ) was synthesized and studied. Compound(Ⅱ) readily reacts with electrophilic reagents, such as hydrogen chloride, acetyl chloride and thionyl chloride, resulting in the cleavage of the oxygen-titanium bond and the formation of compound(Ⅰ).