反应详情

温度

80 °C

3-Bromo-2-methoxy-5-methyl-pyridine (4.0 g, 19.8 mmol), N-bromosuccinimide (4.45 g, 23.8 mmol), and azobisisobutyronitrile (0.163 g, 0.99 mmol) were combined in benzene (40 mL) and stirred overnight at 80° C. The reaction was stirred for another 24 hours at 80° C., and then additional N-bromosuccinimide (1.8 g, 10.1 mmol), and azobisisobutyronitrile (catalytic) were added. After stirring for another 2 hours at 80° C., the mixture was diluted with H2O and extracted with CH2Cl2. The residue was purified by silica gel chromatography to give 3-bromo-5-bromomethyl-2-methoxy-pyridine.

1. stirringThe reaction was stirred for another 24 hours at 80° C.
2. stirringAfter stirring for another 2 hours at 80° C.
3. extractionextracted with CH2Cl2
4. customThe residue was purified by silica gel chromatography