反应详情

A stirred mixture of 2-bromo-3-methoxy-6-methyl-pyridine (2.00 g, 9.9 mmol), Cu(II) sulfate pentahydrate (2.47 g, 9.9 mmol), and potassium peroxydisulfate (8.03 g, 29.7 mmol) in 80 mL of acetonitrile/H2O (1:1) was heated under reflux. After 1 hour, the dark green mixture was cooled to room temperature and CH2Cl2 was added. The layers were separated and the aqueous layer further extracted with CH2Cl2. The organics were combined, dried (MgSO4), filtered and evaporated. The resulting crude product was purified on silica gel [Biotage, hexane:ethyl acetate (4:1)] to give a white solid (0.51 g, 24% yield).

1. temperaturewas heated
2. temperatureunder reflux
3. customThe layers were separated
4. extractionthe aqueous layer further extracted with CH2Cl2
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. customThe resulting crude product was purified on silica gel [Biotage, hexane:ethyl acetate (4:1)]