反应详情

温度

60 °C

To a stirred solution of toluene-4-sulfonic acid 7-(2-fluorophenyl)pyrazolo[1,5-d][1,2,4]triazin-2-yl ester (82.0 mg, 0.213 mmol) in 1,4-dioxane (4 ml) and water (0.8 ml) was added aqueous 4 N NaOH solution (0.270 ml, 1.08 mmol). The solution was heated at 60° C. for 3 h, then the solvents were removed in vacuo. The residue was dissolved in water (10 ml) and washed with ethyl acetate (10 ml). The aqueous layer was acidified to pH<3 and extracted with dichloromethane (6×25 ml). The combined organic extracts were dried (Na2SO4) and evaporated in vacuo to leave 40.7 mg (83%) of the title compound; 1H NMR (360 MHz, d6-DMSO) δ 6.34 (1H, s), 7.42-7.48 (2H, m), 7.71 (1H, m), 7.79 (1H, td, J 7.2 and 1.7 Hz), 9.40 (1H, s), 11.74 (1H, s).

1. customthe solvents were removed in vacuo
2. dissolutionThe residue was dissolved in water (10 ml)
3. washwashed with ethyl acetate (10 ml)
4. extractionextracted with dichloromethane (6×25 ml)
5. dry with materialThe combined organic extracts were dried (Na2SO4)
6. customevaporated in vacuo