反应详情

温度

100 °C

To a round-bottom flask was added a mixture of methyl 2-bromo-4-methylbenzoate (2.00 g, 7.86 mmol, 1.00 equiv) in AcOH (20 mL). I2 (2.45 g, 9.65 mmol, 1.10 equiv), NaIO4 (950 mg, 4.42 mmol, 0.50 equiv), and sulfuric acid (0.1 mL, 0.15 equiv) were added and the resulting mixture was stirred at 100° C. overnight. After cooling to ambient temperature, the reaction was carefully quenched with Na2S2O3 (aq., sat.). The resulting mixture was extracted with 2×50 mL of ethyl acetate. The combined organic layers were dried (Na2SO4) and concentrated in vacuo to yield 2.50 g (81%) of the title compound as an off-white solid.

1. additionTo a round-bottom flask was added
2. temperatureAfter cooling to ambient temperature
3. customthe reaction was carefully quenched with Na2S2O3 (aq., sat.)
4. extractionThe resulting mixture was extracted with 2×50 mL of ethyl acetate
5. dry with materialThe combined organic layers were dried (Na2SO4)
6. concentrationconcentrated in vacuo