反应详情

A solution of 5-bromo-6-(2-methoxyethoxy)-pyridine-2-carboxylic acid (2.48 g, 9 mmol), iodomethane (2.55 g, 18 mmol) and sodium carbonate (0.106 g, 9 mmol) in DMF (30 mL) was stirred overnight at room temperature. The reaction mixture was poured into water and extracted with ethyl acetate (3×50 mL). The combined organic extracts were washed three times with brine, dried (sodium sulfate) and evaporated. The residue was purified by column chromatography (silica gel, 50 g, 30% ethyl acetate in petroleum ether) to yield the title compound (1.7 g, 6 mmol, 65%) as yellow solid; MS (EI): m/e 290.0 [M+H]+.

1. extractionextracted with ethyl acetate (3×50 mL)
2. washThe combined organic extracts were washed three times with brine
3. dry with materialdried (sodium sulfate)
4. customevaporated
5. customThe residue was purified by column chromatography (silica gel, 50 g, 30% ethyl acetate in petroleum ether)