반응 #955955

ord-c044d2a1fa244dfd88caa39a2fce939c

반응 방정식

CC(=O)OC(C)=O
acetic anhydride
CCCCOC(=O)C(C)=O
butyl pyruvate
CC(=O)OC(C)=O
acetic anhydride
C=C(OC(C)=O)C(=O)OCCCC
butyl α-acetoxyacrylate
수율 67.1%

반응 조건

온도
120°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    기타to obtain a second reaction solution
  3. 3
    기타was removed from the second reaction solution
  4. 4
    workup.DISTILLATIONThereafter, the residue was purified by reduced pressure distillation (2 mmHg, 56 to 63° C.)

실험 절차

Next, in a mixture of the obtained butyl pyruvate (235 g, 1.6 mol) and acetic anhydride (333 g, 3.3 mol), p-toluenesulfonic acid monohydrate (5 g) was added. Then, the mixture was stirred under a nitrogen gas stream at 120° C. for 25 hours to obtain a second reaction solution. Next, acetic acid generated by a reaction with excess acetic anhydride under reduced pressure (5 mmHg) was removed from the second reaction solution. Thereafter, the residue was purified by reduced pressure distillation (2 mmHg, 56 to 63° C.) to obtain butyl α-acetoxyacrylate (200 g, yield 67%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08968975B2uspto-grants-2015_03