13423-60-4

288-88-0

591-50-4

13423-60-4

1. CuI (0.10 g, 0.50 mmol), 1,2,4-triazole (0.69 g, 10 mmol), K3PO4 (4.4 g, 20 mmol), iodobenzene (1.4 mL, 12 mmol), and N,N'-dimethylethylenediamine (0.11 mL, 1.0 mmol) were dissolved in DMF (5 mL) under argon protection. Mixed well and degassed. 2. The reaction mixture was heated and stirred at 110°C for 72 hours. 3. 3. After completion of the reaction, the reaction mixture was filtered through diatomaceous earth and the filter cake was washed with ethyl acetate (AcOEt). 4. The solvent was removed by pressurized distillation to give the crude product. 5. The crude product was purified using silica gel column chromatography with heptane/ethyl acetate (7:3, v/v) as eluent. 6. 1-Phenyl-1H-1,2,4-triazole (2a) was isolated in 96% yield as a yellow powder with a melting point of 48 °C (literature value 28-46 °C). 7. The structure of the product was confirmed by 1H NMR and 13C NMR: 1H NMR (CDCl3, 300 MHz) δ 7.42 (m, 1H), 7.53 (m, 2H), 7.71 (m, 2H), 8.15 (s, 1H), 8.74 (s, 1H); 13C NMR (CDCl3, 75 MHz) δ 120.1 (2CH) , 128.3 (CH), 129.9 (2CH), 137.1 (C), 140.9 (CH), 152.7 (CH).