反应详情

To a solution of 3-methyl-2-nitroanisole (10.00 g, 59.8 mmol) in ethanol (60 mL)-tetrahydrofuran (60 mL) is added a 10% palladium on carbon (50% wet, 2.00 g), and the mixture is subjected to hydrogenation, and stirred at room temperature for 1.5 hour. After the reaction is completed, the reaction solution is filtered through celite, and the solvent is evaporated under reduced pressure. To a solution of the residue in ethyl acetate (110 ml) is added acetic anhydride (9.0 mL, 95.2 mmol), and the mixture is refluxed for 5 hours. The reaction solution is cooled with ice, and the precipitated solid is collected by filtration, and washed with hexane to give the title compound (9.28 g, yield: 87%).

1. filtrationthe reaction solution is filtered through celite
2. customthe solvent is evaporated under reduced pressure
3. temperaturethe mixture is refluxed for 5 hours
4. temperatureThe reaction solution is cooled with ice
5. filtrationthe precipitated solid is collected by filtration
6. washwashed with hexane