反应详情

温度

23 °C

To a solution of 4-(8-{4-[2-(3-Chloro-phenyl)-2(S)-hydroxy-ethylamino]-2-oxo-1,2-dihydro-pyridin-3-yl}-6-methyl-9H-purin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (72 mg, 0.124 mmol) in CH2Cl2 (30 mL) was added benzenesulfonyl fonctionalized silica gel, 0.79 meq/g (7.2 g). The heterogeneous mixture was stirred at 23° C. for 16 hours. The solvent was removed by filtration and the silica gel was washed with a mixture of ammonia 2N in MeOH:CH2Cl2 (1:1, 20 mL). The ammoniac solution was evaporated in vacuo to give the title compound as a light yellow solid. (0.053 g, 89%). HPLC 98%; LCMS (+ESI, M+H+) m/z 481; IR (KBr, cm−1) 3262, 2922, 1646, 1597, 1489, 1232; 1H NMR (400 MHz, DMSO+D2O) δ 10.80 (br s, 1H), 7.59-7.29 (m, 5H), 6.23 (d, J=8.2 Hz, 1H), 5.00 (br t, 1H), 3.75 (br s, 4H), 3.62 (m, 1H), 2.89 (br s, 4H), 2.60 (s, 3H); HRMS calcd for C23H25ClN8O2: 480.1789; found 480.1804.

1. customThe solvent was removed by filtration
2. washthe silica gel was washed with a mixture of ammonia 2N in MeOH:CH2Cl2 (1:1, 20 mL)
3. customThe ammoniac solution was evaporated in vacuo