Abstract Optically pure samples of both enantiomers of methyl 2, 3-dihydroxy-2- methylpropanoate were prepared by a chromatographic separation of their (−)-menthyl esters followed by hydrolysis and methylation. Their absolute stereochemistries were established by conversion into their 3-O-acetyl derivatives, compounds of established configuration. NMR and CG-MS methods of determining the optical purities of the diols are ...