反应详情

温度

85 °C

A mixture of 54 (1.30 g, 4.62 mmol), Zn(CN)2 (1.08 g, 9.24 mmol), Pd(PPh3)4 (0.53 g, 0.46 mmol) and NMP (15 mL) was stirred under nitrogen at 85° C. for 14 h. The mixture was filtered and the filtrate was purified by reverse phase chromatography eluting with 35% MeCN/H2O (containing 0.5% ammonia) to afford 0.75 g (70%) 1-(tetrahydro-2H-pyran-2-yl)-1H-benzo[d]imidazole-4-carbonitrile (56) as brown solid: MS (ESI) m/z=228.3 [M+l]+.

1. filtrationThe mixture was filtered
2. customthe filtrate was purified by reverse phase chromatography
3. washeluting with 35% MeCN/H2O (containing 0.5% ammonia)