反应详情

温度

80 °C

To a solution of trifluoromethanesulfonic acid 5-fluoro-2-nitrophenyl ester (4.0 mmol) in DME (10 mL) are added phenylboronic acid (4.8 mmol), Pd(PPh3)4 (0.4 mmol), and K3PO4 (3.2 mmol) at room temperature. After stirring at 80° C. for 6 h, the reaction mixture is filtered through celite, and the filter cake is washed with AcOEt. The filtrate is diluted with water and extracted with ether (×2). The combined organic extracts are dried over Na2SO4, filtered, and concentrated in vacuo. The residue is purified by silica gel column chromatography (n-hexane:AcOEt=6:1) to give the title compound; 1H NMR (CDCl3), δ 7.12-7.19 (2H, m), 7.29-7.32 (2H, m), 7.42-7.45 (3H, t), 7.94 (1H, dd).

1. filtrationthe reaction mixture is filtered through celite
2. washthe filter cake is washed with AcOEt
3. additionThe filtrate is diluted with water
4. extractionextracted with ether (×2)
5. dry with materialThe combined organic extracts are dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe residue is purified by silica gel column chromatography (n-hexane:AcOEt=6:1)