反应 #1925214

ord-9a2cef41679a44e58179eb31c54cfe65

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to terminate
  2. 2
    其他the reaction
  3. 3
    萃取The reaction mixture was extracted with ethyl acetate
  4. 4
    洗涤The organic layer was then washed with water
  5. 5
    干燥dried over anhydrous sodium sulfate
  6. 6
    浓缩After concentration under reduced pressure
  7. 7
    workup.DISTILLATIONthe residue was purified by distillation under reduced pressure

实验过程

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%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06673511B1uspto-grants-2004_01