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General Procedure To a solution of α-halo compound 1 (1.0 mmol, NaN3 (1.2 mmol, and terminal acetylene (1.0 mmol) in aq PEG 400 (2 mL) was added sodium ascorbate (19.8 mg, 10 mol, and 1 M CuSO 4 (50 μL, 5 mol, solution. The reaction mixture was allowed to stir at r.t. for 30 min. After the reaction was complete, as indicated by TLC, the solid product was filtered, washed, and dried to afford pure product. Analytical Data for Selected Compounds Compound 2a:7c IR (KBr, 1690 (CO) cm-1. 1H NMR (200 MHz, CDCl 3, δ, 8.04-8.00 (2 H, m, 7.95 (1 H, s, 7.89-7.84 (2 H, m, 7.73-7.65 (1 H, m, 7.59-7.31 (5 H, m, 5.91 (2 H, s, 13C NMR (50 MHz, CDCl3, δ, 195.0 (CO, 152.4, 139.0, 138.2, 134.5, 133.5, 133.2, 132.7, 132.5, 130.1, 126.4, 59.9. MS EI, m/z calcd for C 16H14N3O [M, H, 264.1; found: 264
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+: 342.0; found: 342.0.
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