反应详情

温度

80 °C

2-Bromo-5-(4-methanesulfonyl-phenoxy)-pyridine (0.47 mmol), sodium-tert.-butylate (1.4 eq.), and 1-methyl-1H-pyrazole-3-amine (1.2 eq.) are dissolved in degassed dioxane (2.5 ml) and heated to 80° C. Chloro(di-2-norbornylphosphino)(2-dimethylaminoferrocene-1-yl)palladium (II) (5.9 mg) in degassed dioxane (1 ml) is added and the reaction mixture is heated for 1 hour at 142° C. in the microwave. The reaction is quenched with ethylacetate (30 ml) and filtrated over celite. The solvent of the filtrate is removed in vacuo [5-(4-Methanesulfonyl-phenoxy)-pyridine-2-yl]-(1-methyl-1H-pyrazole-3-yl)-amine (“A27”) is obtained after reversed phase column chromatography (water/acetonitrile+0.1% TFA) as orange powder in a yield of 55%; HPLC (method C): 1.57 min; LC-MS (method A): 0.787 min, 345.15 (M+H+);

1. temperaturethe reaction mixture is heated for 1 hour at 142° C. in the microwave
2. customThe reaction is quenched with ethylacetate (30 ml)
3. filtrationfiltrated over celite
4. customThe solvent of the filtrate is removed in vacuo [5-(4-Methanesulfonyl-phenoxy)-pyridine-2-yl]-(1-methyl-1H-pyrazole-3-yl)-amine (“A27”)
5. customis obtained after reversed phase column chromatography (water/acetonitrile+0.1% TFA) as orange powder in a yield of 55%
6. custom1.57 min
7. custom0.787 min, 345.15 (M+H+)