The-,-radiation (Co-60) initiated addition of aldehydes to maleates and fumarates gives acylsuccinates identical with those obtained with peroxide initiation. The reaction has been extended for the first time to additions with isobutyraldehyde and to the addition of aldehydes to acetylenedicarboxylates. Both radiral and radiation initiation give products having a 2 3-diacyl structure from the acetylenedicarboxylates.