反应详情

温度

100 °C

To a solution of methyl 4-cyclobutylbenzoate (compound 9.1, 2.00 g, 10.5 mmol) in acetic acid (30 mL) was carefully added sodium periodate (1.00 g, 4.68 mmol), iodine (3.00 g, 11.8 mmol) and sulfuric acid (0.15 g). The resulting mixture was stirred overnight at 100° C. After cooling to room temperature, the reaction was then carefully quenched with saturated aqueous Na2S2O3 (30 mL) and the resulting mixture was extracted with ethyl acetate (3×20 mL). The combined organic layers were washed with brine (3×20 mL), dried (Na2SO4), filtered, and concentrated under reduced pressure to yield of the title compound as a yellow oil (1.50 g, 45%).

1. temperatureAfter cooling to room temperature
2. customthe reaction was then carefully quenched with saturated aqueous Na2S2O3 (30 mL)
3. extractionthe resulting mixture was extracted with ethyl acetate (3×20 mL)
4. washThe combined organic layers were washed with brine (3×20 mL)
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure to yield of the title compound as a yellow oil (1.50 g, 45%)