反应详情

A mixed solution of 4-chloro-3-nitrotoluene (1.30 g) and N,N-dimethylethylenediamine (1.34 g) in 1-propanol (20 ml) was refluxed for 24 hours and the solvent was distilled off under reduced pressure. The residue was dissolved in ethyl acetate and the solution was successively washed with water (×2) 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=30:1) to give 0.19 g of N-(4-methyl-2-nitrophenyl)-N',N'-dimethylethylenediamine.

1. distillationthe solvent was distilled off under reduced pressure
2. dissolutionThe residue was dissolved in ethyl acetate
3. washthe solution was successively washed with water (×2) 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=30:1)