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This paper presents a simplified method for the chemical synthesis of cholest‐4‐en‐3‐one, which is a naturally occurring steroid and a salient intermediate in steroid chemistry. Pyridinium chlorochromate (PCC) in refluxing benzene has been found to be an effective and convenient reagent for the oxidation and concomitant isomerization of cholest‐5‐en‐3β‐ol (cholesterol) to cholest‐4‐en‐3‐one in high yield. Also described are the carbon‐13 nuclear magnetic resonance spectral properties of cholest‐4‐en‐3‐one and of the isolated reaction intermediate cholest‐5‐en‐3‐one.

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