反应详情

Ethyl 2-chlorobenzylcarbamate (809.9 mg) and 2-chloro-3,5-dinitrobenzotrifluoride (932.3 mg) were dissolved in tetrahydrofuran (20 ml), and to the solution was added sodium hydride (151.6 mg) under ice-cooling. The reaction mixture was heated at reflux for 5 hours. After allowing to cool, to the reaction mixture was added 1N hydrochloric acid (200 ml), and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate solution, and then saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by silica gel column (100 g, hexane:ethyl acetate=5:1) to give the title compound (0.286 g, 19%).

1. temperaturecooling
2. temperatureThe reaction mixture was heated
3. temperatureat reflux for 5 hours
4. temperatureto cool, to the reaction mixture
5. extractionthe mixture was extracted with ethyl acetate
6. washThe organic layer was washed with saturated aqueous sodium bicarbonate solution
7. dry with materialsaturated brine, dried over anhydrous magnesium sulfate
8. concentrationconcentrated in vacuo
9. customThe resultant residue was purified by silica gel column (100 g, hexane:ethyl acetate=5:1)