反应详情

温度

55 °C

To a solution of 4-[1-(2-aminopyrimidin-4-yl)-3-methylindazol-6-yl]-2-[1-(oxan-2-yl)-1,2,4-triazol-3-yl]but-3-yn-2-ol (60 mg, 0.13 mmol) in methanol (3 mL) was added p-toluenesulfonic acid (25.38 mg, 0.15 mmol). The reaction mixture was stirred at 55° C. for 1 hr, and then concentrated in vacuo. The crude residue was partitioned between saturated NaHCO3 solution (2 ml) and DCM (2×5 ml). The combined organic extracts were washed with brine (2 mL), dried (Na2SO4), filtered and concentrated in vacuo. The crude product was purified by flash chromatography (Isolute column, 2-10% methanol gradient in DCM) to give the title compound: 1H NMR (500 MHz, DMSO) delta 1.92 (3H, s), 2.58 (3H, s), 6.96 (2H, s), 7.05 (1H, d, J=5.5 Hz), 7.46-7.28 (1H, m), 7.85 (1H, d, J=8.2 Hz), 8.26 (1H, d, J=5.5 Hz), 8.86 (1H, s), 14.01 (1H, s); LC-MS: m/z=+361.05 (M+H)+.

1. concentrationconcentrated in vacuo
2. customThe crude residue was partitioned between saturated NaHCO3 solution (2 ml) and DCM (2×5 ml)
3. washThe combined organic extracts were washed with brine (2 mL)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe crude product was purified by flash chromatography (Isolute column, 2-10% methanol gradient in DCM)