反应详情

温度

100 °C

In a two-neck flask was placed 3,6-dichloropyridazine (1.49 g, 10 mmol), 1-methylpyrazole-4-boronic acid pinacol ester (1.04 g, 5 mmol), K2CO3 (1.38 g, 10 mmol), and Pd(PPh3)4 (289 mg, 0.25 mmol). The resulting mixture was degassed and refilled with N2 (3 times). 1,4-Dioxane/H2O (9 mL/2 mL) was added and the resulting mixture was heated at 100° C. for 5 h. The resulting mixture was poured into EtOAc/H2O (30 mL/30 mL). The organic layer was washed with brine (30 mL), dried (Na2SO4), and filtered. The solvent was removed and the resulting residue was purified by column using 90-100% EtOAc/hexane as the eluent to yield 3-chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine.

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 (9 mL/2 mL) was added
5. additionThe resulting mixture was poured into EtOAc/H2O (30 mL/30 mL)
6. washThe organic layer was washed with brine (30 mL)
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. customThe solvent was removed
10. customthe resulting residue was purified by column