Atropisomeric C2-chiral biaryldiamine ligand, dibenzo[d,f][1,3]-dioxepin-1,11-diamine (H2L, 1) and its platinum amido-bridged tetranuclear complex [(mu-L)2Pt4Me4(mu-Me2S)2] (2) were prepd. and characterized. The diamine 1 was successfully resolved with (+)-tartaric acid; however, the free diamine undergoes substantial racemization within 2 h. Reaction of 2-iodo-3-nitrophenol with methylene iodide and Ullmann intramol. coupling of the produced 1,1'-[methylenebis(oxy)]bis[2-iodo-3-nitrobenzene] afforded 1,11-dinitro-dibenzo[d,f][1,3]dioxepin, characterized by single-crystal x-ray anal. The title diamine 1 was obtained by redn. of the dinitro deriv. with hydrazine hydrate. A test on the coordinating ability of the diamine has produced a complex 2, its crystal structure was detd.

Synthesis and resolution of 1,11-diamino-dibenzo[d,f][1,3]dioxepine: a route to new asymmetric ligands and their complexes / Panunzi, Barbara; Tuzi, Angela; Tingoli, Marco. - In: INORGANIC CHEMISTRY COMMUNICATIONS. - ISSN 1387-7003. - STAMPA. - 13:(2010), pp. 153-156. [10.1016/j.inoche.2009.10.039]

Synthesis and resolution of 1,11-diamino-dibenzo[d,f][1,3]dioxepine: a route to new asymmetric ligands and their complexes.

PANUNZI, BARBARA;TUZI, ANGELA;TINGOLI, MARCO
2010

Abstract

Atropisomeric C2-chiral biaryldiamine ligand, dibenzo[d,f][1,3]-dioxepin-1,11-diamine (H2L, 1) and its platinum amido-bridged tetranuclear complex [(mu-L)2Pt4Me4(mu-Me2S)2] (2) were prepd. and characterized. The diamine 1 was successfully resolved with (+)-tartaric acid; however, the free diamine undergoes substantial racemization within 2 h. Reaction of 2-iodo-3-nitrophenol with methylene iodide and Ullmann intramol. coupling of the produced 1,1'-[methylenebis(oxy)]bis[2-iodo-3-nitrobenzene] afforded 1,11-dinitro-dibenzo[d,f][1,3]dioxepin, characterized by single-crystal x-ray anal. The title diamine 1 was obtained by redn. of the dinitro deriv. with hydrazine hydrate. A test on the coordinating ability of the diamine has produced a complex 2, its crystal structure was detd.
2010
Synthesis and resolution of 1,11-diamino-dibenzo[d,f][1,3]dioxepine: a route to new asymmetric ligands and their complexes / Panunzi, Barbara; Tuzi, Angela; Tingoli, Marco. - In: INORGANIC CHEMISTRY COMMUNICATIONS. - ISSN 1387-7003. - STAMPA. - 13:(2010), pp. 153-156. [10.1016/j.inoche.2009.10.039]
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11588/381679
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