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Radical reaction of o‐substituted arynes with TEMPO and cyclization to bisalkoxyamines. Yields represent isolated yields. Reaction time t=1–18 hours. Conditions: [a] Method A: 4 (0.20 mmol, 1.0 equiv), TEMPO (1.0 mmol, 5.0 equiv), CsF (0.60 mmol, 3.0 equiv), 18‐crown‐6 ether (0.60 mmol, 3.0 equiv), and n‐hexane (2.0 mL). [b] Method B: 4 (0.20 mmol, 1.0 equiv), TEMPO (1.0 mmol, 5.0 equiv), CsF (0.60 mmol, 3.0 equiv), and MeCN (2.0 mL). [c] Reaction was performed on 0.25 mmol scale.
