反应详情

温度

80 °C

To a solution of 6-chloro-2-methyl-3-nitropyridine (0.5 g, 2.9 mmol) in DMF (5 mL) was added Cs2CO3 (1.9 g, 5.8 mmol) followed 3-fluoroazetidine (0.64 g, 5.8 mmol) and the reaction mixture was heated for 2 h at 80° C. The reaction mixture was then diluted with EtOAc and the organic layer was washed with saturated aqueous sodium bicarbonate solution. The organic layer was then dried over sodium sulphate and concentrated. The crude material obtained was purified by column chromatography (silica: 100-200 mesh, MeOH:DCM 2-3%) to afford the title compound (0.6 g, 92%). LCMS (ES+) 211.95 (M+H)+, RT 2.33 minutes (method 1).

1. washthe organic layer was washed with saturated aqueous sodium bicarbonate solution
2. dry with materialThe organic layer was then dried over sodium sulphate
3. concentrationconcentrated
4. customThe crude material obtained
5. customwas purified by column chromatography (silica: 100-200 mesh, MeOH:DCM 2-3%)