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S4 [a] A solution of phenylacetylene (0.60 mmol), p-toluenesulfonyl azide (0.50 mmol), additive (0.60 mmol except entries 1, 14, and 15), and CuI (0.05 mmol) in solvent (1.0 mL) was stirred for 12 h at the indicated temperature.[b] NMR yield based on an internal standard (1, 3-benzodioxole).[c] 0.1 Equiv of sodium ascorbate was employed.[d] Ratio of H2O/t-BuOH was 1: 2.[e] 0.2 Equiv of 2, 6-lutidine was used.