A chiral aluminum solvating agent (CASA) was demonstrated to be a general and efficient reagent for ¹H NMR chiral analysis of alcohols. The sodium salt of the CASA (CASA-Na) showed a complete baseline peak separation of the hydroxyl group for various chiral alcohols including primary, secondary, and tertiary alcohols with alkyl and aryl substituents in CD₃CN. Due to the weak intermolecular interaction, ¹H NMR measurement at low temperature (−40 to 10 °C) was required.