4-Oxoaldehydes, which are important intermediates for the syntheses of terpenoids and jasmonoids, are prepared from the reaction of nitroalkane with acrolein catalyzed by tertiary-phosphine as tributylphosphine, tricyclohexylphosphine or triphenylphosphine, followed by Nef reaction of the resulting 4-nitro aldehyde ethylene acetals. The Michael reaction of nitroethane (1 a) with acrolein was carried out using a variety of tertiary-phosphines as catalysts in benzene at room temperature. Acetalization