反应详情

To a 0° C. mixture of 2,6-dichloro-3-nitropyridine (12 g, 62 mmol) and potassium carbonate (17.1 g, 1.24 mmol) in acetonitrile (200 mL) was added 3-amino pentane by syringe over 30 minutes. After stirring overnight at room temperature, the reaction was concentrated in vacuo. The residue was dissolved in EtOAc and water and the organic layer was washed twice with water and once with brine, dried over sodium sulfate, filtered and concentrated in vacuo. Silica gel chromatography (5%-35% EtOAc/Hexanes) provided the title compound as a yellow solid (7.3 g, 48%). m/z=244.1 (M+H)+

1. concentrationthe reaction was concentrated in vacuo
2. dissolutionThe residue was dissolved in EtOAc
3. washwater and the organic layer was washed twice with water and once with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo