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The structures of the diastereomeric salts of (R)-(ϩ)-and (S)-(Ϫ)-3-(p-chlorophenyl)glutaramic acid with (S)-(Ϫ)-phenylethylamine have been determined by X-ray crystallography. Solubility and melting behaviours of the salts were analysed and correlated with their structural properties in the solid state. The (R)-(ϩ)-3-(p-chlorophenyl)glutaramic acid was converted to (R)-(Ϫ)-baclofen via a Hofmann degradation (57% yield, 99.8% ee, enantiomeric excess).

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