反应详情

温度

130 °C

A 25 mL scintillation vial was charged with 4-tert-butyl-N-(6-chloro-2-hydrazinocarbonyl-pyridin-3-yl)-benzenesulfonamide (691 mg, 1.8 mmol), trimethyl orthoacetate (0.35 mL, 2.8 mmol), ethylamine (5 mL, 2.0 M), AcOH (3.0 mL), and dioxane (10 mL). The vial was sealed, heated to 130° C., and stirred for three hours. The volatiles were then evacuated in vacuo and the residue was purified via automated silica gel chromatography and then preparative HPLC to afford 4-tert-butyl-N-[6-chloro-2-(4-ethyl-5-methyl-4H-[1,2,4]triazol-3-yl)-pyridin-3-yl]-benzenesulfonamide as a white powder: MS (ES) M+H expected 434.1, found 434.1.

1. customThe vial was sealed
2. customThe volatiles were then evacuated in vacuo
3. customthe residue was purified