反应详情

温度

80 °C

To a solution of 6-(1-chloroisoquinolin-4-yloxy)nicotinonitrile (Preparation 17) (300 mg, 1.1 mmol) in DMF (8 mL) under argon was added trimethylboroxine (148 μL, 1.1 mmol) followed by K2CO3 (442 mg, 3.2 mmol) and palladium tetrakistriphenylphosphine (123 mg, 0.1 mmol). The mixture was purged with argon for 5 min and then heated to 80° C. for 16 h. Solvent was removed in vacuo. The residue was partitioned between EtOAc (100 mL) and water (40 mL), the organic phase was washed with water (40 mL), NaHCO3 (40 mL), brine (30 mL) and dried (MgSO4). Solvent was removed in vacuo and the residue purified by column chromatography (2% MeOH: DCM) to give the title compound: RT=2.40 min; m/z (ES+)=262.4 [M+H]+.

1. customThe mixture was purged with argon for 5 min
2. customSolvent was removed in vacuo
3. customThe residue was partitioned between EtOAc (100 mL) and water (40 mL)
4. washthe organic phase was washed with water (40 mL), NaHCO3 (40 mL), brine (30 mL)
5. dry with materialdried (MgSO4)
6. customSolvent was removed in vacuo
7. customthe residue purified by column chromatography (2% MeOH: DCM)