反应详情

To a mixture of 5-chloro-4-(6-iodo-1H-indazol-1-yl)pyrimidin-2-amine (170 mg, 0.46 mmol) and piperidine (1.2 mL) was added tetrakis(triphenylphosphine)palladium (52.9 mg, 0.05 mmol), copper(I) iodide (8.7 mg, 0.05 mmol) and 2-(1,3-thiazol-2-yl)but-3-yn-2-ol (I-1) (140.2 mg, 0.92 mmol). The reaction was purged with N2 and stirred at RT for 20 min. The reaction mixture was concentrated in vacuo and the resultant residue purified by flash chromatography (Isolute column, 1% MeOH in DCM), followed by reverse phase preparative HPLC to give the title compound as a solid: 1H NMR (500 MHz, DMSO) δ 1.91 (3H, s), 7.09 (1H, s), 7.23-7.39 (3H, m), 7.69 (1H, d, J=3.36 Hz), 7.78 (1H, d, J=3.20 Hz), 7.90 (1H, d, J=8.24 Hz), 8.17 (1H, d, J=0.76 Hz), 8.43-8.53 (2H, m); LC-MS: m/z=+397.40 (M+H)+.

1. customThe reaction was purged with N2
2. concentrationThe reaction mixture was concentrated in vacuo
3. customthe resultant residue purified by flash chromatography (Isolute column, 1% MeOH in DCM)