反应详情

温度

100 °C

A mixture of 4-bromo-6-methyl-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole (1.1 g, 3.74 mmol), Zn(CN)2 (873 mg, 7.46 mmol), and Pd(PPh3)4 (646 mg, 0.56 mmol) in NMP (25 mL) under nitrogen was heated at 100° C. overnight. After it was cooled to RT, the reaction mixture was partitioned between EtOAc (300 mL) and water (50 mL). The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by silica gel chromatography using petroleum ether:EtOAc (10:1) as eluting solvents to afford 6-methyl-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole-4-carbonitrile as white solid (400 mg, 50%). MS (ESI): m/z=242.3 [M+1]+.

1. temperatureAfter it was cooled to RT
2. customthe reaction mixture was partitioned between EtOAc (300 mL) and water (50 mL)
3. washThe organic layer was washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by silica gel chromatography
7. washas eluting solvents