反应详情

Ethyl 2-chlorophenylcarbamate (62.6 mg) was dissolved in diglyme (1 ml), and to the solution were added sodium hydride (12.6 mg) and 2-chloro-3,5-dinitrobenzotrifluoride (77.1 mg). The reaction mixture was stirred at room temperature for 1 hour. To the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution, and then saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by preparative TLC (2 mm, 20×20 cm, hexane:ethyl acetate=3:1) to give the title compound (114.8 mg, 93%).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution
3. dry with materialsaturated brine, dried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe resultant residue was purified by preparative TLC (2 mm, 20×20 cm, hexane:ethyl acetate=3:1)