Реакция #955953

ord-8145e7bb54f94012b03842a0a38f85ab

Уравнение реакции

CC(=O)OC(C)=O
acetic anhydride
CCOC(=O)C(C)=O
ethyl pyruvate
CC(=O)OC(C)=O
acetic anhydride
C=C(OC(C)=O)C(=O)OCC
ethyl α-acetoxyacrylate
Выход 58.5%

Растворители

Условия реакции

Температура
120°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas added
  2. 2
    Другоеto obtain a reaction solution
  3. 3
    Другоеwas removed from the reaction solution
  4. 4
    workup.DISTILLATIONThereafter, the residue was purified by reduced pressure distillation (35 to 40 mmHg, 90 to 103° C.)

Методика

First, to a mixture of ethyl pyruvate (315 g, 2.7 mol) and acetic anhydride (554 g, 5.4 mol), p-toluenesulfonic acid monohydrate (8 g) was added. Then, the mixture was stirred under a nitrogen gas stream at 120° C. for 24 hours to obtain a reaction solution. Next, acetic acid generated by a reaction with excess acetic anhydride under reduced pressure (40 to 50 mmHg) was removed from the reaction solution. Thereafter, the residue was purified by reduced pressure distillation (35 to 40 mmHg, 90 to 103° C.) to obtain ethyl α-acetoxyacrylate (250 g, yield 58%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08968975B2uspto-grants-2015_03