Aliphatic aldehyde polyoxyethylene glycol acetals were synthesised through the reaction of aliphatic aldehydes such as caproic aldehyde, capryl aldehyde, capric aldehyde and lauric aldehyde with excess diethylene glycol, triethylene glycol and tetraethylene glycol, respectively. The acetal formation, in which water was azeotropically distilled by adding benzene to the reaction system, was gained a good yield of acetal type compounds. This reaction is found pseudo first order reaction at various temperatures such 70, 80, 90 and 97℃. Also these activation energies of reaction of acetal type products such as caproic aldehyde diethylene glycol acetal, capryl aldehyde diethylene glycol acetal, capric aldehyde diethylene glycol acetal, lauric aldehyde diethylene glycol acetal, caproic aldehyde triethylene glycol acetal and caproic aldehyde tetraethylene acetal were 17.3, 19.6, 21.2, 21.6, 15.5 and 14.7 Kcal/mole.