反应详情

To a solution of 3-bromo-5-hydroxy-benzoic acid (2.0 g, 9.25 mmol), PyBroP (7.7 g, 18.5 mmol) and diisopropylethylamine (6.4 mL, 37 mmol) in DMF (50 mL) was added dimethylamine hydrochloride (1.51 g, 18.5 mmol). The reaction mixture was stirred at room temperature for 6 h. The reaction mixture was diluted with ethyl acetate and washed with brine. The organic extract was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crude material was purified by column chromatography (Isco™ 120 g) using ethyl acetate as eluting solvent to give the title compound (1.5 g, 67%) as a white solid.

1. washwashed with brine
2. extractionThe organic extract
3. dry with materialwas dried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe crude material was purified by column chromatography (Isco™ 120 g)
6. washas eluting solvent