Abstract: | The syntheses of 2,2′‐bithiazole‐containing and related expanded macrocycles 13 – 16 were accomplished by the McMurry coupling reaction of the corresponding 2,2′‐bithiazole]‐5,5′‐dicarbaldehyde 6c and 2,2′‐(1,4‐phenylene)bisthiazole‐5‐carbaldehyde] 7 , readily available by a two‐step reaction sequence. The success of the dimerization strongly depends on the steric repulsion of the substituents vicinal to the CHO group. |