The first unsymmetrical phosphorus(III)-containing macrocycle having hydroquinone and pyrocatechol fragments, N,N,N',N'-tetraethyl-2,4,11,13-tetraoxa-3,12-diphosphatricyclo[12.2.2.0(5,10)]octadeca-1(16),5,7,9,14,17 hexaene-3,12-diamine, was synthesized in a stepwise mode from hexaethylphosphorous triamide, hydroquinone, and pyrocatechol. The product was converted into the corresponding P,P'-dioxide and P,P'-disulfide.