反应详情

温度

0 °C

A mixture of 2,6-dichloro-3-nitropyridine (1.9 g, 10 mmole) and potassium carbonate (1.66 g, 12 mmole) in 30 ml of tetrahydrofuran was stirred at 0° C. for 5 min. A solution of dimethylamine/tetrahydrofuran (2M, 6 ml, 12 mmole) was added dropwise to the reaction mixture over 40 min. After stirring for 5 min at 0° C., the mixture was warmed to room temperature and stirred overnight. The reaction mixture was filtered and the filtrate was collected and concentrated under reduced pressure. The crude product was purified by flash chromatography, eluting with 87% hexane: 13% ethyl acetate to give 6-chloro-2-dimethylamino-3-nitro pyridine (1.05 g).

1. stirringAfter stirring for 5 min at 0° C.
2. temperaturethe mixture was warmed to room temperature
3. stirringstirred overnight
4. filtrationThe reaction mixture was filtered
5. customthe filtrate was collected
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified by flash chromatography
8. washeluting with 87% hexane