反应详情

To a stirred solution of toluene-4-sulfonic acid 7-(2-fluorophenyl)-4-methylpyrazolo[1,5-d][1,2,4]triazin-2-yl ester (3.39 g, 8.51 mmol) in 1,4-dioxane (150 ml) and water (30 ml) was added 4 N aqueous NaOH (10.64 ml, 42.6 mmol) and the mixture was stirred at room temperature for 4 h. The mixture was concentrated in vacuo to about 30 ml, and the aqueous residue was diluted with water (150 ml) and washed with ethyl acetate (50 ml). The remaining aqueous layer was acidified to pH 5 with 5 N aqueous HCl (4 ml) and the resulting precipitate was collected by filtration, washed with water and dried at 60° C. under vacuum to leave 1.98 g (95%) of the title compound as a cream solid: 1H NMR (360 MHz, DMSO-d6) δ 2.68 (3H, s), 6.38 (1H, s), 7.41-7.47 (2H, m), 7.66-7.77 (2H, m); MS (ES+) m/e 245 [M+H]+.

1. concentrationThe mixture was concentrated in vacuo to about 30 ml
2. additionthe aqueous residue was diluted with water (150 ml)
3. washwashed with ethyl acetate (50 ml)
4. filtrationthe resulting precipitate was collected by filtration
5. washwashed with water
6. customdried at 60° C. under vacuum