反应详情

To a solution of 5.00 g (33 mmol) of 3,5-dimethyl-4-methoxyaniline and 7.1 ml of triethylamine in 50 ml of dichloromethane was dropwise added a solution of 4.31 g (40 mmol) of methoxyacetylchloride in 20 ml of dichloromethane under chilling with ice for a period of 30 min. The resulting mixture was stirred for 30 min. at room temperature. The reaction mixture was washed sequentially with 5 aqueous sodium carbonate and 3 N hydrochloric acid, and then dried over anhydrous sodium sulfate. Dichloromethane was distilled off. The residue was crystallized from ether hexane to obtain 6.70 g of the desired compound as a white crystal. (Yield: 90.7 %)

1. temperatureunder chilling with ice for a period of 30 min
2. washThe reaction mixture was washed sequentially with 5 aqueous sodium carbonate and 3 N hydrochloric acid
3. dry with materialdried over anhydrous sodium sulfate
4. distillationDichloromethane was distilled off
5. customThe residue was crystallized from ether hexane