反应详情

温度

100 °C

To a solution of 53 mg of 4-bromo-1H-pyrazolo[4,3-c]pyrid-3-ylamine in 6 mL of dioxane are added 127 mg of 1-(2-fluoro-5-trifluoromethylphenyl)-3-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]urea, 60 mg of sodium bicarbonate in 1.8 mL of water and 30 mg of tetrakis(triphenylphosphine)palladium. The reaction is heated in a bath at 100° C. for 2 hours. The mixture is allowed to cool and ethyl acetate is then added. The mixture is washed with water. The organic phase is dried over magnesium sulfate and then concentrated under reduced pressure. The oily residue is purified on a prepacked Biotage KP-Sil column of 60 Å SiO2 32-63 μm (gradient: 90/10 to 70/30 dichloromethane/solution A; solution A=38/17/2 dichloromethane/methanol/aqueous ammonia). 34 mg of 1-[4-(3-amino-1H-pyrazolo[4,3-c]pyrid-4-yl)phenyl]-3-(2-fluoro-5-trifluoromethylphenyl)urea are obtained in the form of a cream-coloured solid, the characteristics of which are as follows:

1. temperatureto cool
2. washThe mixture is washed with water
3. dry with materialThe organic phase is dried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe oily residue is purified on a prepacked Biotage KP-Sil column of 60 Å SiO2 32-63 μm (gradient: 90/10 to 70/30 dichloromethane/solution A; solution A=38/17/2 dichloromethane/methanol/aqueous ammonia)