反应 #3285036
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06916593B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: At 20 to 30° C., acetic anhydride was added to a mixture of 9.29 g of N,N-bis(2-hydroxyethyl)-2-(methoxycarbonyl)ethylamine, 12.8 g of triethylamine, 50 mg of 4-dimethylaminopyridine and 50 ml of THF and the resulting mixture was stirred for 20 hours. Water was added to terminate the reaction. The reaction mixture was extracted with ethyl acetate. The organic layer was then washed with water and dried over anhydrous sodium sulfate. After concentration under reduced pressure, the residue was purified by distillation under reduced pressure, whereby 13.2 g of N,N-bis(2-acetoxyethyl)-2-(methoxycarbonyl)ethylamine was obtained (boiling point: 118 to 123° C./21 Pa, yield: 99%). to terminate the reaction The reaction mixture was extracted with ethyl acetate The organic layer was then washed with water dried over anhydrous sodium sulfate After concentration under reduced pressure the residue was purified by distillation under reduced pressure
来源 ID: ord-b59d167dff424546b752913c02d0af4c