反应详情

温度

130 °C

In a 10 ml reaction vessel were dissolved 60 mg (0.203 mmol) 3-Bromo-6-methyl-pyridine-2-carboxylic acid (1-methyl-1H-pyrazol-3-yl)-amide and 25 mg (0.254 mmol, 1.5 equiv.) of 3-Amino-1-methyl-pyrazole in 4 ml of dioxane. Cesium carbonate (93 mg, 0.285 mmol, 1.4 equiv.) were added and argon was bubbled through the suspension for 3 min. Then Xanthphos (39 mg, 0.067 mmol, 0.33 equiv.) and Pd2(dba)3.CHCl3 (21 mg, 0.020 mmol, 0.1 equiv.) were added. The vessel was closed and the mixture was heated overnight at 130° C. To the mixture was added silicagel (5 g) and the mixture was evaporated to dryness in vaccuo. The powder was charged onto a silicagel flash chromatography column and eluted (gradient 100% heptane to 100% ethyl acetate) to yield the title compound as a yellow solid (total 11 mg, 17%), MS (ISP): m/e=312.1 (M+H+).

1. customIn a 10 ml reaction vessel
2. customargon was bubbled through the suspension for 3 min
3. customThe vessel was closed
4. additionTo the mixture was added silicagel (5 g)
5. customthe mixture was evaporated to dryness in vaccuo
6. additionThe powder was charged onto a silicagel flash chromatography column
7. washeluted (gradient 100% heptane to 100% ethyl acetate)