Abstract: 3-(β-cyanoethyl)-2-butanone(Ⅰ), 2-(β-cyanoethyl)-cyclohexanone (Ⅱ) and 2-(β-cyanoethyl)-acetophenone (Ⅲ) have been prepared by treating₂-butanone, cyclohexanone and acetophenone respectively with acrylonitrile in the presence of KOH/ethylene glycoi, and converted to corresponding δ-Keto-acids by reflux with dil. HCl . When these δ-Ke-tonic acids are refluxed with ferric sulfate hydrate three unsaturated. lactones that 5,6-dimethyl-3 ,4-dihydro-a-pyrone, △^9,10-hexahydrocoumarin and 6-phenyl-3,4-dihydro-a-pyrone are obtained in yields of 77.8, 86.7 and 29% respectively. Moreover, the (3-Keto-acids above react with alcohols (mothanol, ethanol or butanol) by using hydrated ferric sulfate as catalyst to give (3-Keto-esters in 48-88% yields.