反应详情

温度

8 °C

A suspension of compound (xvii) (10 mg, 0.03 mmol), boronic acid (5.9 mg, 0.04 mmol), cesium carbonate (14 mg, 0.04 mmol) and tetrakis(triphenylphosphine)palladium (2 mg, 0.001 mmol) in ethanol (2 mL) were degassed and stirred under an atmosphere of nitrogen then heated to 8° C. After 3 h the reaction mixture was concentrated and the residue was partitioned between EtOAc (25 mL) and water (15 mL). The organic layer was separated and the aqueous layer was extracted with EtOAc (3×15 mL). The combined organics were washed with brine (15 mL), dried (MgSO4) and concentrated to give 6-(3-aminophenyl)-2-(4-fluorophenyl)-N-methyl-2H-indazole-3-carboxamide (16) (12 mg) as a pale brown oil. The crude material was used directly. ESI-MS m/z calculated for [M+H]+: 361.13; found: 361.14.

1. customwere degassed
2. concentrationAfter 3 h the reaction mixture was concentrated
3. customthe residue was partitioned between EtOAc (25 mL) and water (15 mL)
4. customThe organic layer was separated
5. extractionthe aqueous layer was extracted with EtOAc (3×15 mL)
6. washThe combined organics were washed with brine (15 mL)
7. dry with materialdried (MgSO4)
8. concentrationconcentrated