反应详情

To a solution of 4-bromophenylacetic acid (5.00 g, 23.2 mmol) in tBuOAc (75 mL) was added BF3.OEt2 (2.95 mL, 23.2 mmol). The mixture was allowed to stir overnight at room temperature and poured into H2O. The aqueous phase was extracted with EtOAc. The organic phase was washed with sat. aq NaHCO3, dried over anhydrous Na2SO4, and concentrated in vacuo. Purification by flash chromatography on silica gel (0% to 100% EtOAc in hexanes) provided the title compound. 1H NMR (500 MHz, CDCl3): δ 7.48 (d, J=8.0 Hz, 2 H), 7.19 (d, J=8.0 Hz, 2 H), 3.52 (s, 2 H), 1.48 (s, 9 H).

1. extractionThe aqueous phase was extracted with EtOAc
2. washThe organic phase was washed with sat. aq NaHCO3
3. dry with materialdried over anhydrous Na2SO4
4. concentrationconcentrated in vacuo
5. customPurification by flash chromatography on silica gel (0% to 100% EtOAc in hexanes)