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Extrusion of azobenzene by reductive elimination of 3

BG Benedict M. Gardner
CK Christos E. Kefalidis
EL Erli Lu
DP Dipti Patel
EM Eric J. L. McInnes
FT Floriana Tuna
AW Ashley J. Wooles
LM Laurent Maron
SL Stephen T. Liddle
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Complex 3 was placed in the end bulb of a two bulb sublimation tube and the other bulb was cooled with liquid nitrogen. The reductive elimination product, azobenzene, was collected in the cooled bulb as an orange solid by heating the sample at 100 °C, 4 × 10−6 mbar. Yield: 0.07 g, 26%. Analysis of azobenzene: 1H NMR (C6D6): δ 8.01 (4H, m, CH), 7.17–7.09 (6H, m, CH). GC-MS (ESI positive, MeOH): m/z 182.1 (32%) {PhNNPh}+; (ESI negative, MeOH): m/z 180.97 (64%) {PhNNPh−H+}−.

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