反应详情

温度

60 °C

To a solution of 4,5-dimethoxy-2-nitroaniline (0.81 g) and 2-chloroethyldimethylamine hydrochloride (0.73 g) in N,N-dimethylformamide (20 ml) was added sodium hydride (0.36 g) in small portions with ice-cooling and the reaction mixture was heated at 60° C. for 2 hours. The reaction mixture was diluted with 1N aqueous sodium hydroxide solution and extracted with ethyl acetate. The organic layer was successively washed with water and saturated aqueous sodium chloride solution 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=15:1) to give 0.77 g of N-(4,5-dimethoxy-2-nitrophenyl)-N',N'-dimethylethylenediamine.

1. temperaturecooling
2. extractionextracted with ethyl acetate
3. washThe organic layer was successively washed with water and saturated aqueous sodium chloride solution
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThe solvent was then distilled off under reduced pressure
6. customthe residue was purified by silica gel chromatography (eluent:chloroform:methanol=15:1)