[摘要]：Two- to four-layered [3.3](3,5)pyridinophanes (PyPs) have been synthesized by the (4-tolylsulfonyl)methyl isocyanide (TosMIC) method. The coupling reaction between 3,5-bis[2-isocyano-2-(4-tolylsulfonyl)ethyl]pyridine (TosMIC adduct) and bis(chloromethyl) or tetrakis(bromomethyl) compds. in the presence of NaH in DMF or NaOH and Bu4NI under high-diln. conditions gave the 2-layered dione or 3- and 4-layered tetrones. Wolff-Kishner redn. of the ketones afforded the desired 2- to 4-layered [3.3](3,5)PyPs. The structure of the dione units take an anti geometry whereas the cyclophane units take a syn geometry in soln.
