反应详情

To a solution of 4-cyclobutyl-5-(5-ethoxy-4H-1,2,4-triazol-3-yl)-2-methylbenzonitrile (219.7, 0.15 g, 0.53 mmol) in EtOH (10 ml) was added NH4OH (0.18 ml, 2.66 mmol, 14.8 N in H2O) followed by H2O2 (1.8 ml, 26.6 mmol, 50% in H2O). The mixture was stirred at room temperature overnight. The mixture was cooled to 0° C. and quenched carefully with 1N Na2S2O3 solution (26 ml). The mixture was extracted with EtOAc (×2) and the combined organic layers were dried over Na2SO4, filtered, and concentrated. The residue was purified with prep-TLC (5% MeOH in CH2Cl2). Yield: 0.1 g, white solid, 62.5%. m/z (ES−) 299 (M−H)−.

1. temperatureThe mixture was cooled to 0° C.
2. customquenched carefully with 1N Na2S2O3 solution (26 ml)
3. extractionThe mixture was extracted with EtOAc (×2)
4. dry with materialthe combined organic layers were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified with prep-TLC (5% MeOH in CH2Cl2)