反应详情

In a 100 ml RBF, equipped with a Dean-Stark trap (filled with molecular sieves), was added 5-([1,1′-biphenyl]-3-yl)-3H-1,2,4-triazol-3-amine (1.133 g, 4.80 mmol), dimethyl 2-acetylsuccinate (2.334 mL, 14.39 mmol) followed by Xylene (50 mL) and Ts-OH (9.12 mg, 0.048 mmol). The reaction was heated at reflux for 5 hrs. Filtered and washed by hexanes to collect the off-white solid, which was used directly for the next step. 1H-NMR (500 MHz, CDCl3) δ 2.26 (3H, s), 3.65 (2H, s), 3.72 (3H, s), 7.35-7.36 (1H, m), 7.44-7.46 (2H, m), 7.47-7.48 (1H, m), 7.64-7.66 (2H, m), 7.73-7.75 (1H, m), 8.13-8.15 (1H, m), 8.43 (1 H, s).

1. customIn a 100 ml RBF, equipped with a Dean-Stark trap (filled with molecular sieves)
2. temperatureThe reaction was heated
3. temperatureat reflux for 5 hrs
4. filtrationFiltered
5. washwashed by hexanes
6. customto collect the off-white solid, which