反应详情

To a stirred solution of 9.5 g (0.10 mol) of 2-hydroxypyridine in 250 mL of DMF was added 16.6 g (0.120 mol) of potassium carbonate followed by 25.0 g (0.120 mol) of 2-bromopropionic acid tert-butyl ester. The resulting mixture was stirred at ambient temperature for 7 h then diluted with 1 L of water. The aqueous phase was extracted with ethyl acetate (3×200 mL) and the combined organics were washed with water (2×100 mL), brine (100 mL), dried over magnesium sulfate, filtered and evaporated in vacuo. The crude residue was purified by silica gel chromatography eluting with 25% ethyl acetate in hexanes to afford the title compound as a clear gum 16 g (72%). LC-MS: m/z (ES) 224 (MH)+

1. extractionThe aqueous phase was extracted with ethyl acetate (3×200 mL)
2. washthe combined organics were washed with water (2×100 mL), brine (100 mL)
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customevaporated in vacuo
6. customThe crude residue was purified by silica gel chromatography
7. washeluting with 25% ethyl acetate in hexanes