反应详情

温度

105 °C

A mixture of (6-Bromo-quinoxalin-2-yl)-{(R)-1-[3-(4-methyl-piperazin-1-yl)-phenyl]ethyl}-amine (0.250 g, 1 eq., 0.588 mmol), 1-Boc-4-pyrazole boronic acid pinacol ester (0.190 g, 1.1 eq., 0.647 mmol), caesium carbonate (0.764 g, 4.0 eq., 2.35 mmol) and potassium iodide (0.010 g, 0.1 eq., 0.00588 mmol) in 1,4-dioxane (15 mL) was degassed at RT under vacuum and placed under an atmosphere of nitrogen. The process was repeated twice and Fu's catalyst (Bis(tri-tert-butylphosphine)palladium(0)) (0.015 g, 0.05 eq., 0.029 mmol) was added at room temperature. The reaction mixture was heated at 105° C. in a microwave reactor for 180 minutes. After completion of the reaction (confirmed by TLC), the organic mixture was diluted with ethyl acetate (325 mL) and washed with water (100 mL×3) and brine (100 mL). The organic layer was dried and concentrated under vacuum to give a crude residue.

1. customwas degassed at RT under vacuum
2. additionFu's catalyst (Bis(tri-tert-butylphosphine)palladium(0)) (0.015 g, 0.05 eq., 0.029 mmol) was added at room temperature
3. customAfter completion of the reaction (confirmed by TLC)
4. washwashed with water (100 mL×3) and brine (100 mL)
5. customThe organic layer was dried
6. concentrationconcentrated under vacuum