Five new boronates of the type 2-phenyl-6-aza-1, 3-dioxa-2-borabenzocyclononenes (6a e) were prepared from substituted 2-[(2-hydroxyethylamino) methyl] phenols (4a e) and phenylboronic acid (5) in benzene-EtOH (4: 1) mixtures. Tridentate ligands 4a e and boronates 6a e were characterized by 1H, 13C, 15N, and 2D-NMR (HETCOR, NOESY, and COLOC) experiments, FT-IR, mass spectra, and elemental analysis, as well as 11B NMR ...