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(R)-and S)-4-methyl-[1- 3 H,2- 2 H 1 ]pentanal were prepared from l -and D-leucine via leucic acid and (S)-and (R)-4-methyl-[2- 2 H 1 ]pentanoic acid. Decarbonylation of these samples with tris-(triphenylphosphine)rhodium chloride followed by Kuhn-Roth oxidation of the resulting 2-methylbutane gave chiral acetic acid of 35% e.e. S and 31% e.e. R configuration, respectively. The decarbonylation reaction thus proceeds with net retention of configuration, possibly accom­panied by some racemization.

Steric Course of the Rhodium-Catalyzed Decarbonylation of Chiral 4-M ethyl-[1- 3 H,2- 2 H 1 ]pentanal