反应详情

温度

80 °C

To a mixture of 4-hydroxy-3-(trifluoromethyl)benzoic acid (14.55 mmol) and cesium carbonate (43.7 mmol) in DMA (60 mL) was added 2-bromopropane (36.4 mmol). The reaction was stirred at 80° C. for 16 h. The mixture was filtered through celite and concentrated under vacuum. The residue was dissolved in EtOAc and washed with water, then brine, then dried over MgSO4, and filtered. The solvent was removed under vacuum to give the title compound as a light yellow oil (13.1 mmol). 1H NMR (400 MHz, CDCl3) δ ppm 1.36 (d, J=6.32 Hz, 6H), 1.39 (d, J=6.06 Hz, 6H), 4.72 (septet, J=6.06 Hz, 1H), 5.24 (septet, J=6.25 Hz, 1H), 7.00 (d, J=8.84 Hz, 1H), 7.26 (s, OH), 8.15 (dd, J=8.72, 2.15 Hz, 1H), 8.23 (d, J=2.15 Hz, 1H).

1. filtrationThe mixture was filtered through celite
2. concentrationconcentrated under vacuum
3. dissolutionThe residue was dissolved in EtOAc
4. washwashed with water
5. dry with materialbrine, then dried over MgSO4
6. filtrationfiltered
7. customThe solvent was removed under vacuum