HRID895899
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
PROCEDURE
实验过程
A mixture of 3-bromo-1H-2-pyridone (740 mg, 4.25 mmol), potassium carbonate (1.18 g, 8.5 mmol) and iodomethane (2.65 mL, 42.5 mmol) in DME (10 mL) was heated to reflux overnight. The mixture was filtered, washing with ethyl acetate and the filtrate was evaporated to dryness. The residue was purified by dry column chromatography over 27 g of silica gel, eluting with ethyl acetate to give 3-bromo-1-methyl-2-pyridone (0.63 g, 79%). LRMS (electrospray), positive ion, 188 (M+H).
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux overnight
- filtrationThe mixture was filtered
- washwashing with ethyl acetate
- customthe filtrate was evaporated to dryness
- customThe residue was purified
- customby dry column chromatography over 27 g of silica gel
- washeluting with ethyl acetate