Abstract
An efficient microwave‐assisted synthesis of (±)‐mandelic acid‐d5 was developed. The racemic mixture was resolved by diastereomeric salt formation using 1‐phenylethylamine enantiomers as resolving agents. At each step, the resolution process was checked by determining mandelic acid‐d5 enantiomer ee values directly on fractional crystallized diastereomeric salts by chiral capillary electrophoresis analysis. Highly enriched (−)‐ and (+)‐mandelic acid‐d5 (95% and 90% ee, resp.) were obtained and their absolute configurations—R and S, respectively—were determined by correlation of the (−)‐mandelic acid‐d5 circular dichroism spectrum to the (R)‐mandelic acid one.
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