[摘要]:A robust method for prepg. (3S)-3-alkyl-3-phenyl-1,4-dioxane-2,5-diones, e.g., I, was developed using an improved cyclocondensation reaction between (S)-a-alkylmandelic acids and 2-bromocarbonyl halides. Subtle differences in the reaction conditions, including sep. addns. of triethylamine, significantly increased the yield compared with Schollkopf's original method.