反应详情

To a stirred solution of N-(4-(difluoromethoxy)phenyl)-6-(2-(1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-5-yl)ethyl)pyridazin-3-amine (0.12 g, 0.258 mmol) in DCM (10 mL) was added TFA (1 mL, 12.98 mmol) and the reaction mixture was stirred at room temperature for 3 h. The reaction mixture was concentrated and washed with diethyl ether. The crude product was purified by preparative LCMS on a Waters Xbridge C18 column (19×150 mm, 5 μm) using 0-100% mobile phase B (95:5 Methanol:water with 10 mM NH4OAc) in mobile phase A (5:95 Methanol:water with 10 mM NH4OAc) to give 6-(2-(1H-indazol-5-yl)ethyl)-N-(4-(difluoromethoxy)phenyl)pyridazin-3-amine. 1H-NMR (300 MHz, DMSO-d6) δ ppm 3.07-3.14 (m, 4H) 6.28 (s, 1H) 7.00-7.37 (m, 6H) 7.46 (s, 1H) 7.56 (s, 1H) 7.78 (s, 3H) 7.97 (s, 1H) 9.19 (s, 1H) 12.93 (br. s., 1H).

1. concentrationThe reaction mixture was concentrated
2. washwashed with diethyl ether
3. customThe crude product was purified by preparative LCMS on a Waters Xbridge C18 column (19×150 mm, 5 μm)