Abstract: Diacetoxybutene is prepared by a catalytic reaction of butadiene, acetic acid and oxygen or an oxygen containing gas in the presence of a supported palladium catalyst.In said reaction, the use of butadiene containing vinylcyclohexene in an amount of not more than 5,000 parts by weight per million parts by weight of butadiene and at least one polymerization inhibitor prevents the lowering of the activity of the catalyst thereby prolonging its useful life.