HRID2204336
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of 3-bromo-2-methoxy-5-methyl-pyridine (Step AM3) (3.0 g, 14.7 mmol), was added NBS (3.1 g, 17.6 mmol) and AIBN (121 mg, 0.7 mmol) and the mixture was stirred at 80° C. for 1 h. H2O and CH2Cl2 were added and the phases were separated. The organic layer was dried (MgSO4), filtered and concentrated. The crude product was purified by silica gel column chromatography (heptane/EtOAc, 95:5→0:100). tR: 1.10 min (LC-MS 1).
WORKUP
后处理
- customthe phases were separated
- dry with materialThe organic layer was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was purified by silica gel column chromatography (heptane/EtOAc, 95:5→0:100)