反应详情

温度

0 °C

To a solution of 13 g (73.2 mmol) 2-bromo-3-pyridinol (Fluka 18292) in 40 ml of cone, sulfuric acid 5.1 ml (74 mmol) of nitric acid (65%) are added at 0° C. The reaction mixture is stirred at 0° C. for 12 h, then poured on water and extracted 2× with EtOAc. The combined organic layers are washed with water and saturated NaCl solution, dried over MgSO4, filtered and the filtrate is concentrated in vacuo. The residue is purified by chromatography (silicagel, EtOAc) to afford 5.3 g of 2-bromo-4-nitro-pyridin-3-ol and 2 g of 2-bromo-6-nitro-pyridin-3-ol.

1. additionpoured on water
2. extractionextracted 2× with EtOAc
3. washThe combined organic layers are washed with water and saturated NaCl solution
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationthe filtrate is concentrated in vacuo
7. customThe residue is purified by chromatography (silicagel, EtOAc)