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Trans‐[13,14‐ 14 C 2 ]‐Retinoic acid has been synthesized by condensation of β‐ionylideneacetaldehyde and  14 C‐labeled methyl senecioate in the presence of potassium amide in ether. A convenient synthesis of the key intermediate, methyl (diethoxyphosphinyl)‐[2‐ 14 C]acetate, is also described.