反应详情

温度

100 °C

tert-Butyl {1-[4-(aminocarbonyl)-6-chloropyridin-2-yl]piperidin-4-yl}carbamate (Intermediate 16) (100 mg, 0.282 mmol), copper cyanide (101 mg, 1.13 mmol), Pd(dba) (103 mg, 0.11 mmol) and Dppf (250 mg, 0.45 mmol) were placed in anhydrous dioxane (5 ml) under argon. The mixture was heated at 100° C. for 5 h, then diluted with EtOAc (20 ml) and filtered through celite. The mixture was washed with sodium bicarbonate (2×20 ml), brine (20 ml), dried over sodium sulphate and concentrated in vacuo. The brown residue was purified by flash chromatography eluting with DCM and MeOH mixtures to give the title compound as a brown solid (61 mg).

1. filtrationfiltered through celite
2. washThe mixture was washed with sodium bicarbonate (2×20 ml), brine (20 ml)
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated in vacuo
5. customThe brown residue was purified by flash chromatography
6. washeluting with DCM and MeOH mixtures