The present invention relates to methods for preparing .beta.-ketoester fragrance pro-accords from activated acyl units, 1,3-dioxan-4,6-diones and fragrance raw material alcohols. The first step involves contacting an activated acyl unit, preferably an acid chloride, with a 1,3-dioxan-4,6-dione, an example of which is Meldrum's acid, to form a 2-acyl 1,3-dioxan-4,6-dione which is then reacted with a fragrance raw material alcohol to form the final .beta.-ketoester fragrance pro-accord. The resulting .beta.-ketoester fragrance pro-accords are suitable for use in laundry detergent, personal care, and other formulations wherein aesthetic fragrance materials are employed.