تفاعل #1925214

ord-9a2cef41679a44e58179eb31c54cfe65

معادلة التفاعل

CC(=O)OC(C)=O
acetic anhydride
COC(=O)CCN(CCO)CCO
N,N-bis(2-hydroxyethyl)-2-(methoxycarbonyl)ethylamine
CCN(CC)CC
triethylamine
C1CCOC1
THF
COC(=O)CCN(CCOC(C)=O)CCOC(C)=O
N,N-bis(2-acetoxyethyl)-2-(methoxycarbonyl)ethylamine
المردود 99.0%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىto terminate
  2. 2
    أخرىthe reaction
  3. 3
    استخلاصThe reaction mixture was extracted with ethyl acetate
  4. 4
    غسيلThe organic layer was then washed with water
  5. 5
    تجفيفdried over anhydrous sodium sulfate
  6. 6
    تركيزAfter concentration under reduced pressure
  7. 7
    workup.DISTILLATIONthe residue was purified by distillation under reduced pressure

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06673511B1uspto-grants-2004_01