反应详情

Ethyl 4-chlorophenyl[2,4-dinitro-6-(trifluoromethyl)phenyl]carbamate (1.7323 g) was dissolved in methanol (100 ml), and to the solution was added titanium(III) chloride solution (36.967 g) under ice-cooling. The reaction mixture was stirred for 2 hours. To the reaction mixture was added saturated aqueous sodium bicarbonate solution (800 ml), and the mixture was extracted 2 times with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by silica gel column (70 g, CHCl3:methanol=10:1) to give the title compound (1.2292 g, 82%).

1. temperaturecooling
2. extractionthe mixture was extracted 2 times with ethyl acetate
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe resultant residue was purified by silica gel column (70 g, CHCl3:methanol=10:1)