A novel copper-catalyzed [5 þ 1] annulation of 2-ethynylanilines with an N,O-acetal, which functioned as a C1 part, leading to the preparation of quinoline derivatives with an ester substituent on the 2-position is described. A combination of CuBr 2 and trifluoroacetic acid (TFA) promoting [5 þ 1] annulation of the 2-ethynylaniline with ethyl glyoxylate is also demonstrated.

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Novel mono‐protected catechol derivatives of perhydrophenanthrene are synthesized utilizing hypervalent iodine oxidation and original o‐quinodimethane chemistry of benzocyclobutenes.