反应详情

To a solution of N-(2-nitrophenyl-N',N'-dimethylethylenediamine (1.20 g) in chloroform (25 ml) was added ethyl chloroformate (0.64 g) dropwise. The reaction mixture was stirred at room temperature for 5 hours, washed with 1N aqueous sodium hydroxide solution and saturated aqueous sodium chloride solution in turn and dried over anhydrous sodium sulfate. The solvent was then distilled off under reduced pressure and the residue was purified by silica gel chromatography (eluent:chloroform:methanol=10:1) to give 1.10 g of N-(2-nitrophenyl)-N-ethoxycarbonyl-N',N'-dimethylethylenediamine.

1. washwashed with 1N aqueous sodium hydroxide solution and saturated aqueous sodium chloride solution in turn
2. dry with materialdried over anhydrous sodium sulfate
3. distillationThe solvent was then distilled off under reduced pressure
4. customthe residue was purified by silica gel chromatography (eluent:chloroform:methanol=10:1)