反应详情

温度

80 °C

To 3-[1-(3,5-bis-trifluoromethyl-benzyl)-5-pyridin-4-yl-1H-[1,2,3]triazol-4-yl]-4-(2-chloro-phenyl)-isoxazolo[3,4-d]pyridazine (100 mg, 0.166 mmol), add 8.0 ml of acetonitrile, and 170 μL of water, followed by molybdenum hexacarbonyl (22 mg, 0.083 mmol). Heat the mixture to 80° C. for 4 h., then cool to RT. Pour the mixture through a plug of Celite® (1 cm) and silica gel (2 cm). Concentrate and purify the residue by chromatography (silica gel, hexanes/EtOAc gradient) to provide 42 mg of a yellow solid. Exact Mass 603.1: MS (aspci): m/z=603.9 (M+1), m/z=601.9 (M−1); 1H NMR (300 MHz, CDCl3) δ 8.65–8.80 (m, 3H), 7.79 (s, 1H), 7.65 (br d, J=7.4 Hz, 1H), 7.31 (s, 2H), 7.15–7.00 (m, 2H), 6.96 (d, J=7.4 Hz, 1H), 6.87 (br t, J=7.4 Hz, 1H), 6.12 (br s, 2H), 5.21 (ABq, J=22.5, 7.5 Hz, 2H).

1. temperaturecool to RT
2. additionPour the mixture through a plug of Celite® (1 cm) and silica gel (2 cm)
3. concentrationConcentrate
4. custompurify the residue by chromatography (silica gel, hexanes/EtOAc gradient)