反应详情

A solution of 5-bromo-6-(cyclopropylmethoxy)-pyridine-2-carboxylic acid (Example 9 d, 0.4 g, 1.5 mmol), iodomethane (CAN 16519-98-5, 0.42 g, 3 mmol), sodium carbonate (0.16 g, 1.5 mmol) in DMF (10 mL) was stirred overnight at room temperature. Water was poured into the reaction solution and the resulting mixture was extracted with ethyl acetate (3×30 mL). The combined organic extracts were washed with water and brine, dried over anhydrous sodium sulfate and evaporated. The residue was purified by column chromatography (silica gel, 20 g, 5% ethyl acetate in petroleum ether) to yield the title compound (0.2 g, 0.7 mmol, 48%) as white solid; MS (EI): m/e=286.0 [M+H]+.

1. customwas stirred overnight at room temperature
2. extractionthe resulting mixture was extracted with ethyl acetate (3×30 mL)
3. washThe combined organic extracts were washed with water and brine
4. dry with materialdried over anhydrous sodium sulfate
5. customevaporated
6. customThe residue was purified by column chromatography (silica gel, 20 g, 5% ethyl acetate in petroleum ether)