反应详情

温度

100 °C

In a two-neck flask was placed 1-(1-(6-chloropyridazin-3-yl)piperidin-4-yl)-6-fluoroindoline, prepared as in STEP 3 above (2.33 g, 7 mmol, 1 equiv), 1-methylpyrazole-4-boronic acid pinacol ester (1.75 g, 8.4 mmol, 1.2 equiv), K2CO3 (3.86 g, 28 mmol, 4.0 equiv), and Pd(PPh3)4 (809 mg, 0.7 mmol, 0.1 equiv). The resulting mixture was degassed and refilled with N2 (3 times). 1,4-Dioxane/H2O (30 mL/6 mL) was added and the resulting mixture was heated at 100° C. for 3 h. The resulting mixture was poured into EtOAc/H2O (100 mL/100 mL). The organic layer was washed with brine (100 mL), dried (Na2SO4), and filtered. The solvent was removed by roto-evaporator, and the resulting residue was purified by column using EtOAc as the eluent to yield the title compound as a solid.

1. customIn a two-neck flask was placed
2. customThe resulting mixture was degassed
3. additionrefilled with N2 (3 times)
4. addition1,4-Dioxane/H2O (30 mL/6 mL) was added
5. additionThe resulting mixture was poured into EtOAc/H2O (100 mL/100 mL)
6. washThe organic layer was washed with brine (100 mL)
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. customThe solvent was removed by roto-evaporator
10. customthe resulting residue was purified by column