反应详情

To a solution of the 1-Benzenesulfonyl-5-[4-(2-methylsulfanyl-pyrimidin-4-yl)-1-(tetrahydro-pyran-2-yl)-1H-pyrazol-3-yl]-1H-pyrrolo[2,3-b]pyridine (C-1-2) (750 mg, 1.41 mmol) in MeOH (1 mL) was added a solution of HCl in Dioxane (˜4N, 0.1 mL). After stirring at ambient temperature for 45 minutes, the solution was dropped into phosphate buffer (pH 7, 15 mL). The resulting precipitate was collected by filtration, rinsed with water and air dried to give 5-{4-[2-(methylthio)pyrimidin-4-yl]-1H-pyrazol-3-yl}-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine (C-1-3) (622 mg, 98%) which was carried on without further purification. 1H NMR (400 MHz, ACETONITRILE-d3) δ ppm 11.51 (br. s., 1H), 8.47 (d, J=2.02 Hz, 1H), 8.34 (d, J=5.05 Hz, 1H), 8.23 (br. s., 1H), 8.14 (d, J=7.58 Hz, 2H), 8.10 (d, J=1.77 Hz, 1H), 7.84 (d, J=2.78 Hz, 1H), 7.68 (t, J=7.45 Hz, 1H), 7.57 (t, J=7.71 Hz, 2H), 7.07 (d, J=4.80 Hz, 1H), 6.75 (d, J=3.79 Hz, 1H), 1.81 (s, 3H).

1. filtrationThe resulting precipitate was collected by filtration
2. washrinsed with water and air
3. customdried