反应详情

温度

80 °C

A mixture of 2-bromo-6-{[tert-butyl(dimethyl)silyl]oxy}-1,3-benzothiazole (500 mg, 1.45 mmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-amine (383 mg, 1.2 equiv), aqueous potassium carbonate (2.0 M, 2.9 ml, 4.0 equiv) and Pd(dppf)Cl2 (119 mg, 0.10 equiv) in DMF (6.0 ml) was stirred at 80° C. under argon for 2 h. The mixture was then added to DCM (100 ml), dried (Na2SO4) and concentrated in vacuo. The crude thus obtained was purified by silica gel chromatography by gradient elution (n-heptane:ethyl acetate) to yield 237 mg of the title compound. 1H NMR δ 9.74 (s, 1H) 8.53 (d, 1H) 7.94 (dd, 1H) 7.73 (d, 1H) 7.35 (d, 1H) 6.93 (dd, 1H) 6.61 (s, 2H) 6.55 (d, 1H); MS m/z (M+H) 244.

1. dry with materialdried (Na2SO4)
2. concentrationconcentrated in vacuo
3. customThe crude thus obtained
4. customwas purified by silica gel chromatography by gradient elution (n-heptane:ethyl acetate)