反应详情

3-Bromo-2-hydroxy-5-nitropyridine (8.5 g, 39 mmol) and N,N′-dimethylformamide (0.5 ml) in chloroform (75 ml) were treated dropwise with phosphorous oxychloride (7.3 ml, 80.2 mmol) and heated at reflux for 24 hrs. The mixture was then cooled and concentrated, before being partitioned between ethyl acetate (80 ml) and sodium hydrogen carbonate solution (50 ml). The organic phase was washed with brine (100 ml), dried Na2SO4) and concentrated to give the product as a yellow solid (8.88 g).

1. temperatureheated
2. temperatureat reflux for 24 hrs
3. temperatureThe mixture was then cooled
4. concentrationconcentrated
5. custombefore being partitioned between ethyl acetate (80 ml) and sodium hydrogen carbonate solution (50 ml)
6. washThe organic phase was washed with brine (100 ml), dried Na2SO4) and
7. concentrationconcentrated