Abstract
The unexpected formation of 6‐methyl‐2‐(2‐methylpropenyl)cyclohex‐2‐enone (6) during a deprotecting reaction of 1,3‐dioxane (5) via an interesting carbonyl‐ene reaction at room temperature with original aim to obtain 4,8‐dimethyl‐5‐oxonon‐6‐en‐1‐al (4) is reported. An alternative route to aldehyde (4) is also presented.