反应详情

To a solution of 3-bromo-5-(trifluoromethyl)benzoic acid (12.43 g, 0.04620 mol) in MeOH (200 mL) was added H2SO4 (8 mL). The reaction mixture was heated at reflux overnight and then concentrated to small volume. The residue was extracted with EtOAc and washed with water, brine, aq. sat. NaHCO3, and brine. The organic solution was concentrated to give methyl 3-bromo-5-(trifluoromethyl)benzoate (12.7 g, 92%). 1H NMR (300 MHz, CDCl3) δ: 8.36 (s, 1H), 8.23 (s, 1H), 7.95 (s, 1H), and 3.97 (s, 3H).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux overnight
3. concentrationconcentrated to small volume
4. extractionThe residue was extracted with EtOAc
5. washwashed with water, brine, aq. sat. NaHCO3, and brine
6. concentrationThe organic solution was concentrated