Abstract: The thermally labile di-tert-butyl-, tert-butyl-, and dimethyl-a-peroxylactones la, lb, and IC were readily prepared in 35, 50, and 68% yields, respectively, by dicyclohexylcarbodiimide cyclization of the respective a-hydroperoxy acid 2a, 2b, and 2c in methylene chloride at subambient temperatures. These volatile a-peroxylactones were isolated and purified by low-temperature flash distillation and exhibit a characteristic ...