反应详情

A mixture of 5-bromopyridine-2-carboxylic acid (3.0 g), N,O-dimethylhydroxylamine hydrochloride (2.9 g), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (5.69 g), 1-hydroxybenzotriazole (4.01 g), N,N-diisopropylethylamine (12.97 mL), 4-dimethylaminopyridine (0.181 g) and DMF (37.1 mL) was stirred at room temperature for 5 hr, and water was added. The mixture was extracted with ethyl acetate, and the extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.76 g).

1. extractionThe mixture was extracted with ethyl acetate
2. washthe extract was washed with water and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe solvent was evaporated under reduced pressure
5. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)