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The novel macrocyclic compounds, hexadecahydroxy[(1.0)
8
]- (2c) and hexahydroxy[3.0.1.0.1.0]-metacyclophane (3) are isolated in 1.9 and 2.4% yields, respectively, from the reaction mixture obtained by CsOH-catalysed condensation of 5,5′-di-tert-butyl-2,2′-dihydroxybiphenyl 1 with formaldehyde under xylene reflux.