反应详情

A solution of 2-fluoro-4-(trifluoromethoxy)benzoic acid (3 g, 13.4 mmol), DPPA (4.4 g, 16.1 mmol) and Et3N (1.63 g, 16.1 mmol) in 130 mL of t-BuOH was refluxed for 4 h, and then concentrated. The residue was dissolved in dichloromethane (200 mL), washed with 1M HCl aqueous solution, dried over Na2SO4, and concentrated under reduced pressure. The crude product was purified by flash column chromatography on silica gel (petroether/AcOEt=4/1) to get the title compound (2 g, 50% yield) as a yellow solid: 1H NMR (400 MHz, CDCl3): δ ppm 1.27 (s, 9H), 6.97-7.03 (m, 1H), 7.21-7.27 (m, 1H), 7.37-7.41 (m, 1H).

1. concentrationconcentrated
2. dissolutionThe residue was dissolved in dichloromethane (200 mL)
3. washwashed with 1M HCl aqueous solution
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe crude product was purified by flash column chromatography on silica gel (petroether/AcOEt=4/1)