反应详情

温度

80 °C

To a stirred suspension of 2-[2-amino-6-(4-chloro-phenylamino) pyrimidin-4-yl]-4-bromo-phenol (0.059 g, 0.15 mmol), 4-chloro-benzylchloride (0.073 g, 0.45 mmol) and cesium carbonate (0.098 g, 0.30 mmol) in acetonitrile (10 ml) was added potassium iodide (40 mg). The mixture was stirred at 80° C. for 2 hours. Filtration and concentration of the filtrate provided a crude product which was purified by preparative TLC eluting with ethyl acetate-hexane (1:3) to provide the title compound (0.02 g, 26% yield). 1H NMR (CD3OD) δ 5.23 (s, 1H, CH2), 6.41 (s, 1H, Ar), 7.26 (d, 1H, J=9.6 Hz, Ar), 7.38-7.42 (m, 6H, Ar), 7.71-7.74 (m, 4H, Ar).

1. filtrationFiltration and concentration of the filtrate
2. customprovided a crude product which
3. customwas purified by preparative TLC
4. washeluting with ethyl acetate-hexane (1:3)