反应详情

温度

60 °C

2-Fluoro-4-methyl-5-nitropyridine (0.8 g, 5.12 mmol), tert-butyl piperazine-1-carboxylate (1.05 g, 5.64 mmol) and potassium carbonate (0.85 g, 6.15 mmol) were taken up in acetonitrile (15 mL) and heated at 60° C. for 1.5 h. After this time, the reaction was quenched with water (20 mL) and extracted with EtOAc (2×30 mL). The organic layers were combined and dried over sodium sulphate, then concentrated in vacuo. The crude material was purified by column chromatography (silica gel: 100-200 mesh, 1:1 EtOAc/heptane) to give the title compound (1.57 g, 97%). LCMS (ES+) 323.1 (M+H)+, RT 1.71 minutes (method 4).

1. customAfter this time, the reaction was quenched with water (20 mL)
2. extractionextracted with EtOAc (2×30 mL)
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by column chromatography (silica gel: 100-200 mesh, 1:1 EtOAc/heptane)