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General procedure: To 64.3 mg (0.278 mmol) of TTbQ-Me dissolved in anhydrous acetone (20 ml) in a two necked flask, 30 mg (0.278 mmol) of p-benzoquinone and 120 mg (0.116 mmol) of Pd2DBA3CHCl3 were added in sequence under inert atmosphere (Ar). The resulting mixture was stirred in the dark for 30 min, filtered on a celite filter and evaporated under vacuum to a small volume. Addition of Et2O induces the precipitation of the complex which was filtered off and dried in a desiccator for 5 h. 82.2 mg of the title compound as a red solid were obtained (yield 80percent).
General procedure: Heteroleptic Cu-dipeptide-necuproine complexes where L-dipeptide: Gly-Val, Gly-Leu, <strong>[3321-03-7]Gly-Phe</strong>, Ala-Gly, Ala-Phe, Val-Phe, Phe-Ala or Phe-Phe were obtained as follows (Fig. 1). 0.1mmol of dipeptide were dissolved in the minimum volume of warm water (10-50mL) and 0.1mmol of CuSO4·5H2O was added. The pH was adjusted to 7 with a 0.1M NaOH solution. A solution of 0.1mmol of neo in 5mL of ethanol was added, while stirring. The compounds were isolated by evaporation at 40-50C, until blue crystals were formed. Yield 60-70%. Crystals suitable for X-ray analysis were obtained by slow evaporation of solvent at room temperature.
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