反应详情

A mixture of 2,4-dimethyl-3-hydroxypyridine (3.00 g, 24.36 mmol) and Na2CO3 (5.16 g, 48.7 mmol) in MeOH (40 mL) and water (24 mL) was treated with iodine (6.18 g, 24.36 mmol) and stirred at RT for 1 h. Additional iodine (0.4 g) was added, the mixture stirred at RT for 3 h, then acidified to pH=5 with 3M HCl. The mixture was treated with brine, extracted with EtOAc (2×) and the combined organics were washed with brine, dried over Na2SO4 and concentrated to dryness to afford 6-iodo-2,4-dimethylpyridin-3-ol (5.1 g, 84%). MS (ESI) m/z: 250.0 (M+H+).

1. stirringthe mixture stirred at RT for 3 h
2. extractionextracted with EtOAc (2×)
3. washthe combined organics were washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated to dryness