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a) DSC analysis for 1 a in air; b) Quenching of the fluorescence of [Ru(bipy)3][PF6]2 following the addition of 1 a; c) trapping the postulated diazomethyl radical intermediate with 1,3,5‐trimethylbenzene to afford product 3 a and formation of diethyl acetylenedicarboxylate via radical dimerization and dinitrogen elimination.
