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1,3‐Dipolar cycloadditions to 3‐benzvalenyI phenyl sulfones and elimination of phenylsulfinic acid afforded access to valenes such as 1 and 2. With a synthesis according to Paal and an Aldol condensation according to Hinsberg the benz‐valene‐annelated thiophenes 3 were obtained. The different formal arrangement of the double bonds in 1, on the one hand, and in 2, 3 on the other, give rise to clearly different 13C‐NMR chemical shifts of the bicyclobutane bridgehead atoms.

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Die IH-NMR-Spektren von la und lb in schwach koordinierenden Lösungsmitteln (CD 2 CI 2 , CDCI 3 , [Da]