반응 #955957

ord-506a9d03aa8d4c378f44e32d1cb45819

반응 방정식

CC(=O)OC(C)=O
acetic anhydride
CCCCCCCCOC(=O)C(C)=O
octyl pyruvate
CC(=O)OC(C)=O
acetic anhydride
C=C(OC(C)=O)C(=O)OCCCCCCCC
octyl α-acetoxyacrylate
수율 59.2%

반응 조건

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

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    기타obtaining 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 (1 mmHg or less, 80 to 102° C.)

실험 절차

Next, in a mixture of the obtained octyl pyruvate (300 g, 1.5 mol) and acetic anhydride (306 g, 3.0 mol), p-toluenesulfonic acid monohydrate (5 g) was added. Then, the mixture was stirred under a nitrogen gas stream at 120° C. for 27 hours, thereby obtaining 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 (1 mmHg or less, 80 to 102° C.), thereby obtaining octyl α-acetoxyacrylate (215 g, yield 59%).

출처

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