反应详情

温度

100 °C

To a solution of 2,6-dibromo-4-nitropyridine 1-oxide (6.80 g, 22.82 mmol) in acetic acid (100 mL) at rt was added Fe powder (6.40 g, 114.13 mmol). The resulting reaction mixture was heated to 100° C. for 1 h. After completion of reaction (by TLC), acetic acid was distilled off under reduced pressure, the residue was basified with aqueous ammonia solution and extracted with EtOAc (3×250 mL). The combined organics were washed with brine, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue thus obtained was treated with ether and hexane and filtered to obtain the desired product as an off white solid (5.40 g, 94%).

1. customThe resulting reaction mixture
2. distillationwas distilled off under reduced pressure
3. extractionextracted with EtOAc (3×250 mL)
4. washThe combined organics were washed with brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue thus obtained
9. filtrationfiltered